HRID27246

反应详情

EQUATION

反应方程式

HRID 27246 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

3.6 Parts of lithium aluminum hydride is added to a solution of 10 parts of 2-benzyl-3,4-dihydro-8-phenyl-1(2H)-isoquinolone in 225 parts by volume dry tetrahydrofuran and the resulting mixture is stirred at reflux temperature for about 5 hours. Then the mixture is cooled in an ice bath and treated successively with 7.5 parts by volume of water in 15 parts by volume of tetrahydrofuran, 7.5 parts by volume of 25% sodium hydroxide, and 7.5 parts by volume of water. The salts which form are filtered off and the filtrate is dried over anhydrous magnesium sulfate and concentrated under reduced pressure to yield clear oil. The oil is taken up in ether and treated with isopropanolic hydrogen chloride to give, as a white solid, 2-benzyl-8-phenyl-1,2,3,4-tetrahydroisoquinoline hydrochloride, melting at about 187°-189° C. after recrystallization from a mixture of ethanol and ether. This compound has the following formula ##STR16##

WORKUP

后处理

  1. temperatureat reflux temperature for about 5 hours
  2. temperatureThen the mixture is cooled in an ice bath
  3. filtrationThe salts which form are filtered off
  4. dry with materialthe filtrate is dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customto yield clear oil