Acetyl chloride → (8R,9aR)-8-[(5-cyclopropylpyrazin-2-yl)oxy]octahydro-5H-pyrrolo[1,2-a][1,4]diazepin-5-one hydrochloride

tert-Butyl (8R,9aR)-8-[(5-cyclopropylpyrazin-2-yl)oxy]-5-oxohexahydro-1H-pyrrolo[1,2-a][1,4]diazepine-2(3H)-carboxylate (50 mg, 0.103 mmol, Part A) was dissolved in methanol (1.0 mL) in a 20-mL scintillation vial. In a separate 4-mL vial, acetyl chloride (0.090 ml, 1.29 mmol) was added to methanol (0.5 mL) at 0° C., and the resulting acidic solution was added to the reaction vial. The vial was capped, and the reaction mixture was heated to 60° C. for 0.5 hour. The reaction mixture was then cooled to room temperature and concentrated to provide (8R,9aR)-8-[(5-cyclopropylpyrazin-2-yl)oxy]octahydro-5H-pyrrolo[1,2-a][1,4]diazepin-5-one hydrochloride that was used in the next step without additional purification.

1. additionthe resulting acidic solution was added to the reaction vial
2. customThe vial was capped
3. temperatureThe reaction mixture was then cooled to room temperature
4. concentrationconcentrated

ORDレコード

ord-c854db948682488bb1a9e2e53f90bc67

出典データセット

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09029361B2