HRID6729
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe solvent was evaporated
- dissolutionthe resulting residue was dissolved in water
- extractionextracted 3 times with diethyl ether
- additionThe aqueous layer was neutralized to pH 8 by the addition of potassium hydroxide
- extractionextracted with diethyl ether
- dry with materialThe basic ether layer was dried over sodium sulfate
- customthe solvent was removed in vacuo