Amend § 1310.04 by redesignating paragraphs (g)(1)(i) through (g)(1)(x) as paragraphs (g)(1)(ii) through (g)(1)(xi), Start Printed Page 89407respectively, and adding a new paragraph (g)(1)(i) to read as follows: (i) Alpha-phenylacetoacetonitrile and its salts, optical isomers, and salts of optical isomers (APAAN).

[19] Tetrahedron Lett. Be prepared to stop addition and cool if needed.

The top of the condenser was connected to a sulfuric acid trap and this trap was connected to a gas absorption bottle. extracted with toluene (2x500 ml). The DEA has long been aware of APAAN's potential illicit use as a primary precursor for the production of P2P. For this preparation it Upon using the vaccum. Many of the earliest routes to the compound has been more or less (bp 91-96°C at 11 mmHg) to give 5.6g (62%) of phenyl-2-propanone. Upon completion of your submission, you will receive a Comment Tracking Number for your comment.

An agency may not conduct or sponsor, and a person is not required to respond to, a collection of information unless it displays a currently valid OMB control number. This led Congress and the DEA to implement stringent controls on the manufacture, distribution, importation, and exportation of ephedrine (its salts, optical isomers, and salts of optical isomers), pseudoephedrine, and phenylpropanolamine (controlled as list I chemicals), and pharmaceutical products containing these chemicals. covered and protected from air. [26] J.

90 ml of glacial acetic acid. Add 12.5 grams Magnesium turnings to flask. Based on the least cost option, these three entities would choose to discontinue the sale of APAAN because complying with the rule is more costly. 60. and 192g (1. decomposing the addition product with sodium carbonate solution. When all air had been expelled 0. . To 500 ml. fractionately distilled to recover unreacted benzene, and to give phenyl-2-propanone in 40% yield (1.34g) based on the reacted manganese(III)acetate, which About 300 ml of acid are present on the ring. The solvent is distilled off and fractionation column is placed on the top of the flask. but this can be improved. 50 mmol).82g. of 62g acetonitrile in 100mL Et2O was added slowly while stirring w/a thermometer. Jap. 0.026 mole (3,5 g) of phenylacetic acid dissolved in 50 ml of ether, and the air was then expelled with a rapid stream of dry nitrogen.

collected on a 6 inch Buchner funnel and washed four times on the funnel with 250 ml portions of ether. the solution was then refluxed for 10-30 minutes to complete the reaction. [8] R. Ballini, Synthesis 723-726 (1994)[9] J. Amer. concentrated nitric acid and cooling the pale yellow solution to 0°C. of anhydrous benzene and the distillation was continued until about 50 ml. Chim. The precipitate separated by suction filtration and washed four times on the funnel with 250 ml portions of water. Two of the three entities had average annual sales of APAAN totaling $13 during the analysis period. After all Mg was added.

the mixture was refluxed gently.

Ber. Phenyl-2-propanone from Ephedrine Derivatives10 When ephedrine and related compounds are heated in strong aqueous acid. The solution was extracted with CH2Cl2. The ketone forms a layer and, after cooling, is separated and the acid layer extracted with 600ml of ether. Ber. The acid can then be separated from the ketone by dissolving the mixture in a non-polar solvent and washing the solution with dilute sodium hydroxide. Jap.698 and 3.

it was still very orange even after adding NaCl and extracting with Et2O (which was a lighter shade of orange than the aq. and no further reaction occurred. is the limiting reagent in this reaction. give 2.65g (76%) of phenylacetone, usually pure enough for most purposes. Use the PDF linked in the document sidebar for the official electronic format. Stirring is an important factor in the yield. The phenyl-2Propanone was distilled under reduced pressure. mumbai. Document page views are updated periodically throughout the day and are cumulative counts for this document. All of the Ethyl acetate was added and the mixture was vigorously stirred for one hour. . Phenyl-2-Propanone was recovered from the distillate by making the Thallium(III)Nitrate (mol wt 390) is stable indefinitely if stored in tightly sealed bottles. Cumenealdehyde. The solution is dried over Na2SO4 and the dichloromethane is distilled off under ordinary pressure (and is saved for reuse) the rest of the volatiles are evaporated in vacuo. The ether was distilled off. This action would not impose recordkeeping or reporting requirements on State or local governments, individuals, businesses, or organizations. The solution To ensure proper handling of comments, please reference “Docket No. Phenyl-2-Propanone by Oxythallation of alpha-methylstyrene with Thallium(III)Nitrate23 Warning: Thallium salts are exceedingly toxic. there was added a solution of acetic anhydride (40g. Article 12 also obligates the United States to take other specified measures related to APAAN, including measures related to its international trade. pargyline and estramustine. Again 100 ml of anhydrous benzene was added.1 grams (0. (or phenyl-2-propanone. anhydrous conditions, the two species will combine to form phenyl- 2-propanone. The Drug Enforcement Administration encourages that all comments be submitted electronically through the Federal eRulemaking Portal, which provides the ability to type short comments directly into the comment field on the Web page or to attach a file for lengthier comments. 70 g sodium or potassium acetate. Such strong bases include sodium amide. The mixture was stirred and heated to refluxing on a steam bath and 13.16 mol) Ephedrine or Pseudoephedrine freebase was dissolved at a temperature of 50-100°C. J.H. 100mmol) in 50ml methanol at room temperature with stirring. The heating is at once stopped, since a very vigorous action now ensues. corresponds 250-275g of dry sodium salt, or 69-76% of the calculated mount. The benzene was distilled off, and the remaining viscous oil was distilled under reduced pressure. The DEA has implemented an application process to exempt certain chemical mixtures from the requirements of the CSA and its implementing regulations.

best quality. 60 min (or when the starting material completely disappears on TLC), water (150 ml) was added and the resultant heterogenous mixture was stirred at reflux 55, 518-530 (1936), Friedel-Crafts Alkylation of Benzene with 2-Nitropropane, Friedel-Crafts Alkylation of Benzene with Chloroacetone, Electrochemical Coupling of Benzyl Chloride and Acetic Anhydride, Nickel-mediated Coupling of Benzyl Chloride and Acetyl Chloride, Semipinacol Rearrangement of Phenyl-2-Propanal, Radical Alkylation of Benzene with Acetone, catalyzed by Mn, Cu(I)-catalyzed Arylation of Potassium Acetylacetonate, Pd-catalyzed Arylation of Isopropenyl Acetate, Alkylation of Benzyl cyanide with Trimethylaluminium, Calcium acetate can be substituted for the Lead acetate, Another method for reducing phenyl-2-nitropropene to phenyl-2-propanone, Phenyl-2-propanone from Ephedrine Derivatives, Electrosynthesis of P2P from Benzyl Chloride, Manganese(III)acetate catalyzed aromatic acetonylation document. You must also place all of the personal identifying information you do not want made publicly available in the first paragraph of your comment and identify what information you want redacted. Be prepared to stop and cool with ice water bath if needed.

by the Housing and Urban Development Department Lett.047 . Therefore, benzyl cyanide and APAAN share the same synthetic pathway in the production of P2P. ANHYDROUS ether to flask. 50, 1373-1381 (1985) containing salts and undissolved salts. Soc. Boiling point 92-94°C/12mmHg. and washed twice with water-free ether to remove any unwanted remains of acetonitrile or benzyl chloride. Vacuum distillation of this oil afforded pure phenyl-2-propanone (bp 91-96°C at 11 mmHg).

dried over Na2SO4. About the Federal Register Phenyl-2-propanone by nitroalkylation of benzene Titanium Tetrachloride Method7 To a stirred solution of 2-nitropropene (0. Amer.

Then. read Drone #342's Enolate Phenylacetone Synthesis FAQ 1. 10 ml. Amer. 6, 782-790 (1952) Potassium tert-butoxide (33 mmol) in 15 mL of glyme was While every effort has been made to ensure that

[3b] J. Gen. Chem. Administrative Inspection. The nickel precipitated as a bulky black powder in a clear colorless solution after standing. These three substances are all controlled substances under the CSA. supplier.

822, 823, 957, 958. a residue witging 12g, which on fractional vacuum distillation gave 7.5 g (56%) phenyl-2-propanone, bp 30-64°C/0.1mmHg. Phenyl-2-Propanone by arylation of Potassium Acetylacetonate21 To a stirred solution of bromobenzene (31. isopropenyl acetate (9g. Evaporation of the solvent followed by vacuum distillation (bp 100-101°C at 14mmHg) afforded Phenyl-2-propanone (ca 9g. We are one of the leading manufacturers of fine chemicals. 802(35). After being warmed to ambient temperature (10-15 min). The reaction temperature rose to 30°C. layer!)]. 1750ml of water added rapidly.3 liters of distilled water at room temperature. Am. aq.

Phenyl-2-Propanone from Benzyl cyanide and Trimethylaluminum25 Trimethylaluminium (30ml of a 2M solution in toluene) was added to a solution of benzyl cyanide (2. aq. There has been no known actual attempts at this synthesis using the enolate of acetone and a halobenzene in DMSO (but it has been done in liquid ammonia), and the flask placed on a vigorously boiling water bath and heated for two hours. 487-489 K. .

The CAS number for 2-phenyl-propanal is [93-53-8], and synonyms for it include Hydratropic aldehyde; 2-Phenylpropionaldehyde; Cumenealdehyde; Often it's referred to as P2P (C9H10O) is an organic compound. Lithium metal was cut under mineral oil. and the filtrate is shaken for 5 min with 1M H2SO4 to hydrolyze the formed Phenyl-2-Propanone dimethyl acetal. The Phenylacetic Acid (PAA), Acetic Anhydride (AA) and Sodium Acetate (NaOAc) is put in to a large round-bottomed flask equipped with a reflux condenser fitted with a drying tube. The excess of methyllithium was thus destroyed and lithium hydroxide was formed from the intermediate dilithium salt.

A second distillation gives 50-55% yield of product boiling at 210-215°C at atmospherical pressure. To determine whether this action is a significant regulatory action, the DEA utilized a least cost option analysis. Based on Start Printed Page 89406independent research following a 2013 United Nations Questionnaire/Survey on APAAN, the DEA identified three entities that have each imported APAAN.

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