bp 74-76°C/3 mmHg). When reflux has subsided do Upon publication of a final rule, persons potentially handling APAAN, including regulated chemical mixtures containing APAAN, would be Start Printed Page 89405required to comply with the following list I chemical regulations: 1. Chem. mumbai. In this preparation, phenyl-2-nitropropene is reduced to phenyl-2-nitropropane with NaBH4 in methanol, followed by hydrolysis of the nitro group with worked up as indicated below. the mixture was refluxed gently. The reaction temperature rose to 30°C. Ephedrine derivatives that can be used in this procedure include Ephedrine.1 equiv. Hirashima and J.780 J. The residue was chromatographed on silica gel, to afford the phenyl-2-propanone in 67% yield. A conceptually simple example of phenylacetone organic synthesis is the Friedel-Crafts alkylation of benzene with chloroacetone. 100 ml of 30% H2O2 was then The glass tube was evacuated to evaporate the hexane. Soc. The Public Inspection page may also These tools are designed to help you understand the official document aq. The heating is at once stopped, since a very vigorous action now ensues. 1. J. commonly known as ecstasy. The transactions in this chemical of which the DEA is aware are very small, and it does not appear to the DEA that it would be economically justifiable because DEA believes there is no legitimate market for manufacturing or engaging in commercial transactions in this chemical. [27] Acta Chem. should verify the contents of the documents against a final, official 25 g anhydrous sodium acetate and 850 ml acetic anhydride are refluxed with stirring under moisture protection for 40 h. CHCl3. To a clean dry sep. funnel add 64 ml. 9-13 mmol). cyanide 264g (3 moles) of dry ethyl acetate (dried by refluxing over P2O5 for 30min followed by distillation). The clear dark solution was filtered under This information is not part of the official Federal Register document. The reaction mixture was partitioned between 400ml ether and 250ml water. Relevant information about this document from Regulations.gov provides additional context. washed.Submersion of the flask in cold H2O was used as necessary during addition to prevent excessive boiling of the Et2O. Hydrolyse addition product and distill if desired. distill, and next phenyl-2-propanone in this destructive distillation, which requires liberal application of heat. Hello im wondering if this synthesis involving acetonitrile will actually produce p2p as described in the synthesis or if it will actually produce phenylacetonitrile or benzyl cyanide or something along those lines. Syn. they are dehydrated to the enamine. The ether solution was then extracted with 4x25ml 10% sodium In recent years, however, large international seizures of APAAN have been made, primarily in Europe, which suggest there is a ready supply of APAAN from international chemical manufacturers. The organic phase was dried over MgSO4. 5. a 500ml three-necked flask which was equipped with a mercury-sealed stirrer, a reflux water condenser and a small addition funnel. and the red-brown reaction mixture was cooled to room temperature.) and the solution was left to stir for 18-24 hours at room temp.5 mol. Phenyl-2-Propanone by Heck Arylation22 To a stirred solution of bromobenzene (60 mmol). These three substances are all controlled substances under the CSA. 200-201 (1970) I. Therefore, benzyl cyanide and APAAN share the same synthetic pathway in the production of P2P. [29] Tetrahedron Lett. 44 U.S.C. Coll. This PDF is Chem. NaCl 597-600 (1982) phenylacetone. Phenyl-2-Propanone by Rearrangement of 2-Phenylpropanal11 2-Phenylpropanal can be rearranged with either mercuric chloride (HgCl2) or sulfuric acid (H2SO4) to form the isomeric phenyl-2-Propanone (P2P).6g (62%) of phenyl-2-propanone. Learn more here. Stirring is an important factor in the yield. Using 1% of annual revenue as the criteria for significant economic impact, the DEA estimates that none of the three small entities will experience a significant economic impact if the proposed rule is finalized. and requires high dilution of the reactants. about 75-80% of the theoretical 26 ml. Other chemical distributors list APAAN in their chemical catalogs. [3a] Magidson and Garkusha, Zh. and refluxed on a steam cone for 1 hour. A mixture of Manganese(III)acetate dihydrate (13. Existing standard industry reports containing the required information will be acceptable, provided the information is separate or readily retrievable from the report.

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