HRID1284257

反应详情

EQUATION

反应方程式

HRID 1284257 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Methylmercapto-5H-dibenzo[a,d]cyclohepten-5-one, 27.9 g. (0.11 mole), is dissolved in 500 ml. of methanol. The solution is stirred and heated to refluxing while a solution of 14.9 g. (0.276 mole) of potassium borohydride in 150 ml. of water containing 0.2 ml. of 10 N. sodium hydroxide is added dropwise. After stirring at reflux for 2 hours, the solution is chilled and the precipitated product collected and washed with methanol yielding, typically, 27 g. (96%). An analytical sample melts at 117°-118.5°C. after repeated recrystallizations from methanol.

WORKUP

后处理

  1. dissolution(0.11 mole), is dissolved in 500 ml
  2. temperatureheated
  3. temperatureto refluxing while a solution of 14.9 g
  4. stirringAfter stirring
  5. temperatureat reflux for 2 hours
  6. temperaturethe solution is chilled
  7. customthe precipitated product collected
  8. washwashed with methanol yielding
  9. customrecrystallizations from methanol