HRID1461470

反应详情

EQUATION

反应方程式

HRID 1461470 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of bis N-(t-butyloxycarbonyl)-cystamine (77.37 g, 0.220 mole) from Example 1, in 1 L of ethanol was treated with NaBH4 (32.5 g, 0.859 mmole). Vigorous gas evolution ensued and subsided in 40 minutes. The reaction was stirred for an additional half hour and was poured into 2.5 L of a cold dilute solution of citric acid (pH 6). The mixture was then extracted with 3×1 L of chloroform. The combined organic extracts were dried with MgSO4 and the solvents were removed under reduced pressure. The resulting residue was distilled (66°-73° C. 0.25 torr) to obtain the product (41.5 g, 53% yield).

WORKUP

后处理

  1. extractionThe mixture was then extracted with 3×1 L of chloroform
  2. dry with materialThe combined organic extracts were dried with MgSO4
  3. customthe solvents were removed under reduced pressure
  4. distillationThe resulting residue was distilled (66°-73° C. 0.25 torr)