反应 #543568

反应方程式

borohydride

4-(tert-Butoxycarbonyl-hydrazono)-piperidine-1-carboxylic acid tert-butyl ester

product A9

4-(tert-Butoxycarbonyl-hydrazono)-piperidine-1-carboxylic acid tert-butyl ester

water

→

4-(N′-tert-Butoxycarbonyl-hydrazino)-piperidine-1-carboxylic acid tert-butyl ester

溶剂

tetrahydrofurane

反应条件

后处理

1. 1
   workup.ADDITIONAfter complete addition
2. 2
   workup.ADDITIONis added
3. 3
   其他to destroy the excess of borohydride
4. 4
   其他Subsequently the tetrahydrofurane is evaporated
5. 5
   萃取the resulting aqeous solution extracted with diethyl ether
6. 6
   干燥After drying the solvent over magnesium sulfate
7. 7
   其他the ether is evaporated

实验过程

150 ml of a solution of borohydride in tertahydrofurane (1.0 mol/l) is slowly added to a solution of 0.12 mole of 4-(tert-Butoxycarbonyl-hydrazono)-piperidine-1-carboxylic acid tert-butyl ester (intermediate product A9) in 100 ml of dry tetrahydrofurane. After complete addition, the mixture is stirred for another 30 min after which a 100 ml of water is added to destroy the excess of borohydride. Subsequently the tetrahydrofurane is evaporated and the resulting aqeous solution extracted with diethyl ether. After drying the solvent over magnesium sulfate, the ether is evaporated. M. p.112–115° C.

来源