HRID2071744
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
3-Methylmercapto-5H-dibenzo[a,d]cyclohepten-5-one, 2.9 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
- dissolution(0.11 mole), is dissolved in 500 ml
- temperatureheated
- temperatureto refluxing while a solution of 14.9 g
- stirringAfter stirring
- temperatureat reflux for 2 hours
- temperaturethe solution is chilled
- customthe precipitated product collected
- washwashed with methanol yielding
- customrecrystallizations from methanol