Hydrochloric Acid → (+-)-p-Methoxyamphetamine

HRID 275419

반응식

HRID 275419 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9](=O)C)=[CH:5][CH:4]=1.[C:12]([O-])(=O)C.[NH4+].[C:17]([BH3-])#[N:18].[Na+].Cl>CO>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH:17]([NH2:18])[CH3:12])=[CH:5][CH:4]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 74764'-MethoxyacetophenoneHCID 517165Ammonium AcetateHCID 5003444Sodium cyanoborohydride

생성물 1

HCID 31721(+-)-p-Methoxyamphetamine

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 32 g (0.21 mol) of 4'-methoxyacetophenone and 165 g (2.1 mol) of ammonium acetate in 450 ml of methanol is combined with 13.5 g (0.21 mol) of sodium cyanoborohydride, which is added in batches thereto at ambient temperature, with stirring. After a further 20 hours, ice is added and the mixture is acidified with hydrochloric acid (conc. HCl H2O=1/1) until the pH is 2. The acidic solution is extracted with dichloromethane. The aqueous phase is then mixed with conc. ammonia, with cooling, until a clearly alkaline reaction occurs and then extracted exhaustively with dichloromethane. The combined dichloromethane extracts are dried over sodium sulphate and evaporated to dryness in vacuo. The crude 2-(4-methoxyphenyl)-1-methylethylamine thus obtained is purified by column chromatography over silica gel (eluant: dichloro-methane/methanol=20/1) to remove any by-products. A colorless oil is obtained which can be used for reaction without any further purification.

후처리

  1. additionis added in batches
  2. additionice is added
  3. extractionThe acidic solution is extracted with dichloromethane
  4. additionThe aqueous phase is then mixed with conc. ammonia
  5. temperaturewith cooling, until a clearly alkaline reaction
  6. extractionextracted exhaustively with dichloromethane
  7. dry with materialThe combined dichloromethane extracts are dried over sodium sulphate
  8. customevaporated to dryness in vacuo

출처 및 근거

ORD 기록
ord-ca523392809241f08caa36aabdb2c1c5
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05393774

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