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
CONDITIONS
反应条件
- 温度
- 85 °C
PROCEDURE
实验过程
(R)-1-(4-tert-Butoxyphenyl)ethylamine (89.4 g, 0.463 mol) was dissolved in 10% hydrochloric acid (200 ml) and heated to 85° C. At approx. 80° C., vigorous gas evolution set in. The mixture was stirred at 85° C. for another three hours, after which the gas evolution had stopped. The pale yellow mixture was allowed to cool to room temperature and then 20% NaOH was added dropwise up to a pH of 10.2. The deprotected phenol precipitated out overnight in the form of a pale yellow powder. It was filtered off with suction and dried in a drying cabinet overnight. For purification, the crude product was digested with tert-butyl methyl ether (200 ml). The suspension was filtered and the filter residue was dried again under reduced pressure. 51.3 g (63%) of (R)-4-(1-aminoethyl)phenol were obtained in the form of a pale yellow powder.
WORKUP
后处理
- customAt approx. 80° C.
- temperatureto cool to room temperature
- customThe deprotected phenol precipitated out overnight in the form of a pale yellow powder
- filtrationIt was filtered off with suction
- customdried in a drying cabinet overnight
- customFor purification
- filtrationThe suspension was filtered
- customthe filter residue was dried again under reduced pressure