Dimethylformamide → Ethyl 3-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-2-{[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-carbonyl]-amino}-propionate

温度

0 °C

4.15 g (23.04 mmol) CDT was added to a suspension of 8.00 g (23.04 mmol) ethyl 2-amino-3-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-propionate (Intermediate product 58) and 16.0 mL (115.00 mmol) triethylamine in 100 mL DMF at 0° C. and the mixture was stirred for 1.5 hours at 0° C. A solution of 5.64 g (23.00 mmol) 3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one in 200 mL DMF was added and the mixture was heated to 100° C. for 2 hours. The reaction mixture was cooled to RT, diluted with 1.5 L water and stirred for a further 10 minutes. The precipitate formed was filtered off, washed with water and dried i. vac.

1. temperaturethe mixture was heated to 100° C. for 2 hours
2. temperatureThe reaction mixture was cooled to RT
3. stirringstirred for a further 10 minutes
4. customThe precipitate formed
5. filtrationwas filtered off
6. washwashed with water
7. customdried i

ORDレコード

ord-0f08dae74b384c0c95bfa70330a3865d

出典データセット

uspto-grants-2009_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07538115B2