HRID6729

反应详情

EQUATION

反应方程式

HRID 6729 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-hydroxyphenylacetone (0.5 g, Avocado, U.K.) and ammonium acetate (2.54 g, Aldrich, U.S.A.) in 10 mL methanol was added 0.17 g of sodium cyanoborohydride (Aldrich, U.S.A.). After stirring for 72 h at rt, concentrated hydrochloric acid was added dropwise until the solution reached pH 2. The solvent was evaporated and the resulting residue was dissolved in water, then extracted 3 times with diethyl ether. The aqueous layer was neutralized to pH 8 by the addition of potassium hydroxide and extracted with diethyl ether. The basic ether layer was dried over sodium sulfate and the solvent was removed in vacuo to give 0.23 g of 4-(2-amino-propyl)-phenol.

WORKUP

后处理

  1. customThe solvent was evaporated
  2. dissolutionthe resulting residue was dissolved in water
  3. extractionextracted 3 times with diethyl ether
  4. additionThe aqueous layer was neutralized to pH 8 by the addition of potassium hydroxide
  5. extractionextracted with diethyl ether
  6. dry with materialThe basic ether layer was dried over sodium sulfate
  7. customthe solvent was removed in vacuo