HRID236867

反应详情

EQUATION

反应方程式

HRID 236867 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

0.7 g cis-2-methyl-3,3a,8,12b-tetrahydro-dibenzo[ 1,2;5,6]cyclohepta[3,4-c]pyrrol-1(2H)-one is dissolved in 25 ml dry ether/tetrahydrofuran (1:1). This solution is slowly added at 0° C. to a suspension of 0.35 g LiAlH4 in 20 ml ether/t.h.f. (1:1). After stirring for 15 minutes, water is added and the mixture is then filtered. The filtrate is subsequently evaporated to dryness under vacuum. This gives an oily residue, weighing about 0.7 g. Addition of 8 ml ethanol to this residue results in the formation of a precipitate, which is filtered off. [The crystalline product thus obtained is recrystallized, giving 0.25 g 2-methyl-2,3,3a,8-tetrahydro-dibenzo[ 1,2;5,6]cyclohepta[3,4-c]pyrrole of melting point 128°-131° C. (= enamine according to formula III)].

WORKUP

后处理

  1. filtrationthe mixture is then filtered
  2. customThe filtrate is subsequently evaporated to dryness under vacuum
  3. customThis gives an oily residue
  4. customresults in the formation of a precipitate, which
  5. filtrationis filtered off
  6. custom[The crystalline product thus obtained
  7. customis recrystallized