Hydrochloric Acid → (+-)-p-Methoxyamphetamine

HRID 275419ノート

反応式

HRID 275419 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 31721(+-)-p-Methoxyamphetamine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ca523392809241f08caa36aabdb2c1c5
出典データセット
uspto-grants-1995_02
特許番号
US05393774

反応ノート

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