反応 #162707

反応方程式

diethyl ether

tert-butyl {(1R,2S)-2-[(2-{[(2-methoxyethyl)amino]carbonyl}-6-methylquinazolin-4-yl)amino]cyclohexyl}carbamate

hydrogen chloride-ethyl acetate

→

desired compound

収率 92.0%

4-{[(1S,2R)-2-aminocyclohexyl]amino}-N-(2-methoxyethyl)-6-methylquinazolin-2-carboxamide

収率 92.0%

溶媒

ethyl acetate

反応条件

後処理

1. 1
   workup.ADDITIONwas added
2. 2
   workup.STIRRINGthe mixture was stirred for 30 minutes
3. 3
   ろ過Then, the deposited substance was collected by filtration
4. 4
   洗浄washed with diethyl ether
5. 5
   その他dried under reduced pressure
6. 6
   その他The resulting powder was purified by Fuji Silysia NH silica gel column chromatography (chloroform:methanol=20:1)

実験手順

To a suspension of 2.24 g of tert-butyl {(1R,2S)-2-[(2-{[(2-methoxyethyl)amino]carbonyl}-6-methylquinazolin-4-yl)amino]cyclohexyl}carbamate in 10 ml of ethyl acetate, 10 ml of a 4 N hydrogen chloride-ethyl acetate solution was added, and the mixture was stirred at room temperature for 48 hours. To the reaction solution, 20 ml of diethyl ether was added, and the mixture was stirred for 30 minutes. Then, the deposited substance was collected by filtration, washed with diethyl ether and dried under reduced pressure. The resulting powder was purified by Fuji Silysia NH silica gel column chromatography (chloroform:methanol=20:1), whereby 1.61 g of a desired compound was obtained as a colorless powder.

出典