HRID981988

反应详情

EQUATION

反应方程式

HRID 981988 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

(1R,4R)-5-phenylmethyl-2,5-diazabicyclo[2.2.1] heptane dihydrobromide. A mixture of (1R,4R)-2-(4-toluenesulfonyl)-5-phenylmethyl-2,5-diazabicyclo[2.2.1]heptane (38.95 g, 0.11 mole) in AcOH (500 mL) containing HBr (30% wt) was heated at 70° C. for 18 h. The mixture was allowed to cool and the precipitate that formed was filtered and washed with acetone. The filtrate was concentrated to one-third of the original volume and the resulting solid was combined with the first precipitate to give the title compound (36.55 g, 92%, m.p. 272°-275° C.).

WORKUP

后处理

  1. temperatureto cool
  2. customthe precipitate that formed
  3. filtrationwas filtered
  4. washwashed with acetone
  5. concentrationThe filtrate was concentrated to one-third of the original volume