HRID363697

反应详情

EQUATION

反应方程式

HRID 363697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Silver acetate (1.3 g) was added to a solution of 3-(4-hydroxyphenyl)propylamine hydrochloride (1.2 g) and N,N'-Bis(tert-butoxycarbonyl)-S-methylisothiourea (1.86 g) in DMF (10 mL) containing triethylamine (3.0 g). The mixture was stirred for 3 hr, and an additional 1.0 g silver acetate was added. After one hour, the mixture was diluted with ethyl acetate, filtered through Celite, washed with water, dried over magnesium sulfate, and the solution evaporated. Chromatography on silica gel with 20% ethyl acetate in hexane provided the title compound as a white solid, mp 142°-144° C. (dec) after recrystallization from hexane-ethyl acetate (2.1 g, 77%).

WORKUP

后处理

  1. waitAfter one hour
  2. filtrationfiltered through Celite
  3. washwashed with water
  4. dry with materialdried over magnesium sulfate
  5. customthe solution evaporated