HRID1357790

反应详情

EQUATION

反应方程式

HRID 1357790 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1-(4-Methoxy-benzenesulfonyl)-2,3,4,7-tetrahydro-1H-azepine-2,3-dicarboxylic acid 3-benzyl ester 2-tert-butyl ester (6 g, 12 mmol) is dissolved in a mixture of 120 ml Tetrahydrofuran and 78 ml Water. LiOH·H2O (1 g, 24 mmol) is added. After 45 min., more Water (15 ml) is added and the reaction solution is stirred at room temp. for 24 h. The solvent is evaporated and the remaining solid is resolved in Water/Diethylether. The water layer is acidified to pH 1. The organic phase is separated and the water phase is extracted twice with Ethylacetate. The combined organic fractions are dried with MgSO4 and filtered. The solvent is evaporated to afford the product: Cal. 412.5, found (M)+ 412.1.

WORKUP

后处理

  1. customThe solvent is evaporated
  2. customThe organic phase is separated
  3. extractionthe water phase is extracted twice with Ethylacetate
  4. dry with materialThe combined organic fractions are dried with MgSO4
  5. filtrationfiltered
  6. customThe solvent is evaporated
  7. customto afford the product