反应 #452457

反应方程式

product

Boc-4-aminomethylbicyclo-[2.2.2]octane carboxylic acid

carbonyldiimidazole

H2O

NH4OH

→

title compound

Boc-4-aminomethylbicyclo-[2.2.2]octane carboxamide

溶剂

DMF

反应条件

后处理

1. 1
   其他After 30 min the DMF was evaporated in vacuo
2. 2
   其他to afford 50-60 ml of a light brown paste, which
3. 3
   workup.ADDITIONrapidly added
4. 4
   其他precipitation of product, which
5. 5
   其他was triturated
6. 6
   其他isolated by filtration
7. 7
   洗涤washing with H2O
8. 8
   其他dried in vacuo

实验过程

A stirred solution under N2 of 12.0 g (42.5 mmol) of the product from step B in 100 ml of DMF was treated with 8.0 g (49.3 mmol) of carbonyldiimidazole. After 30 min the DMF was evaporated in vacuo to afford 50-60 ml of a light brown paste, which was stirred and treated with 70 ml of conc. NH4OH rapidly added. The initial solution turned to a white paste within 30 min, after which H2O was added up to a total volume of 400 ml to complete precipitation of product, which was triturated and isolated by filtration and washing with H2O, and dried in vacuo to yield the title compound as a white solid.

来源