反応 #76025

反応方程式

(+)-(2S)-2-amino-3-cyclohexyl-1-propanol

tert-butyl isothiocyanate

→

N-(tert-butyl)-N′-[(1S)-1-cyclohexylmethyl-2-hydroxyethyl]thiourea

溶媒

—

petroleum ether

ethanol

反応条件

後処理

1. 1
   その他After concentration of the reaction mass under reduced pressure (5 kPa) at a temperature in the region of 50° C., the oil obtained
2. 2
   ろ過The crystals are filtered off
3. 3
   その他dried under reduced pressure (10 Pa) at a temperature in the region of 60° C

実験手順

The process is performed as in Example 3, starting with 8.1 g of (+)-(2S)-2-amino-3-cyclohexyl-1-propanol and 9.8 cm3 of tert-butyl isothiocyanate in 79 cm3 of ethanol. The reaction medium is stirred for 72 hours at a temperature in the region of 20° C. After concentration of the reaction mass under reduced pressure (5 kPa) at a temperature in the region of 50° C., the oil obtained is taken up in 110 cm3 of cold petroleum ether. The crystals are filtered off and dried under reduced pressure (10 Pa) at a temperature in the region of 60° C. 11.1 g of N-(tert-butyl)-N′-[(1S)-1-cyclohexylmethyl-2-hydroxyethyl]thiourea are obtained in the form of a white solid melting at 97° C.

出典