反応 #944975

反応方程式

HCl

1-{(2R)-2-[(tert-butoxycarbonyl)amino]-2-cyclohexylethanoyl}-N-[5-chloro-2-(4-chloro-1,2,5-thiadiazol-3-yl)benzyl]-L-prolinamide

→

1-[(2R)-2-Amino-2-cyclohexylethanoyl]-N-[5-chloro-2-(1,2,5-thiadiazol-3-yl)benzyl]-L-prolinamide hydrochloride

溶媒

CH2Cl2

反応条件

後処理

1. 1
   その他The resulting solid was triturated with EtOAc
2. 2
   ろ過filtered

実験手順

HCl gas was bubbled through a stirred 0° C. solution of 1-{(2R)-2-[(tert-butoxycarbonyl)amino]-2-cyclohexylethanoyl}-N-[5-chloro-2-(4-chloro-1,2,5-thiadiazol-3-yl)benzyl]-L-prolinamide (41.1 mg, 0.07 mmol) in CH2Cl2 (1.0 mL) for 15 min. The solution was reduced in vacuo. The resulting solid was triturated with EtOAc and filtered. 1-[(2R)-2-Amino-2-cyclohexylethanoyl]-N-[5-chloro-2-(1,2,5-thiadiazol-3-yl)benzyl]-L-prolinamide hydrochloride was isolated as a solid. 1H NMR (CD3OD 400 MHz) δ 1.30 (m, 6H), 1.74 (m, 2H), 1.86 (m, 4H), 2.02 (m, 2H), 2.23 (m, 1H), 3.62 (m, 1H), 3.75 (m,1H), 3.98 (d, J=6.0 Hz, 1H), 4.42 (m, 1H), 4.64 (s, 2H), 7.46 (dd, J=2.2, 8.2 Hz, 1H), 7.62 (s, 1H), 7.74 (d, J=8.2 Hz, 1H), 8.99 (s, 1H): MS m/z=462.6.

出典