反応 #162706

反応方程式

diisopropyl ether

{(1S,2R)-2-[(tert-butoxycarbonyl)amino]cyclohexyl}amino-6-methylquinazolin-2-carboxylate

2-methoxyethylamine

→

desired compound

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

溶媒

methanol

反応条件

後処理

1. 1
   workup.ADDITIONwas added
2. 2
   温度After the reaction solution was cooled to room temperature
3. 3
   workup.STIRRINGthe mixture was stirred at 0° C. for 30 minutes
4. 4
   ろ過The deposited crystal was collected by filtration
5. 5
   洗浄washed with diisopropyl ether
6. 6
   その他dried under reduced pressure

実験手順

To a suspension of 15.0 g of ethyl 4-({(1S,2R)-2-[(tert-butoxycarbonyl)amino]cyclohexyl}amino-6-methylquinazolin-2-carboxylate in 15 ml of methanol, 7.89 g of 2-methoxyethylamine was added, and the mixture was stirred at 50° C. for 15 hours. After the reaction solution was cooled to room temperature, 45 ml of diisopropyl ether was added thereto, and the mixture was stirred at 0° C. for 30 minutes. The deposited crystal was collected by filtration, washed with diisopropyl ether and dried under reduced pressure, whereby 12.2 g of a desired compound was obtained as a white powder.

出典