Ethyl Acetate → (R)-(-)-2-oxo-3-tert-butoxycarbonylamino-5-phenyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine

温度

145 °C

To a solution of 5 g of (R)-(+)-2-oxo-3-tert-butoxycarbonylamino-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine in 25 ml of cyclohexanone were added 5.96 g of cyclooctene and 0.5 g of 10% palladium carbon. The mixture was stirred at the internal temperature of 145° C. for 2.5 hours. After the reaction mixture was cooled to room temperature, 20 ml of ethyl acetate was added. The mixture was filtered and the filtrate was concentrated under reduced pressure. The residue was crystallized by adding thereto diisopropyl ether and n-hexane and the resulting crystals were collected by filtration, whereby 3.2 g of the title compound was obtained.

1. temperatureAfter the reaction mixture was cooled to room temperature
2. filtrationThe mixture was filtered
3. concentrationthe filtrate was concentrated under reduced pressure
4. customThe residue was crystallized
5. additionby adding
6. filtrationdiisopropyl ether and n-hexane and the resulting crystals were collected by filtration

ORDレコード

ord-cd97a41839564bccb51d26a6e8f7ae1f

出典データセット

uspto-grants-2004_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06747022B2