Water → {(1S,2S,4R)-4-(2,2-Dimethylpropylcarbamoyl)-1-[4-(2,6-difluorophenyl)-2,2-dimethyl-5-oxopiperazin-1-ylmethyl]-2-hydroxypentyl}carbamic acid t-butyl ester

温度

80 °C

8 mg of 2-hydroxypyridine (0.083 mmol) was added to a solution of 200 mg of {(S)-2-[4-(2,6-difluorophenyl)-2,2-dimethyl-5-oxopiperazin-1-yl]-1-[(2S,4R)-4-methyl-5-oxotetrahydrofuran-2-yl]ethyl}carbamic acid t-butyl ester obtained in Example (93b) (0.42 mmol) in (2,2-dimethylpropyl)amine (1 ml), and the mixture was stirred at 80° C. for six hours. The reaction mixture was cooled and then water was added, followed by extraction with methylene chloride. Then, the organic layer was dried over anhydrous magnesium sulfate. After filtration, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (elution solvent:methylene chloride/methanol=40/1-20/1) to obtain 221 mg of the title compound (yield: 94%).

1. temperatureThe reaction mixture was cooled
2. extractionfollowed by extraction with methylene chloride
3. dry with materialThen, the organic layer was dried over anhydrous magnesium sulfate
4. filtrationAfter filtration
5. customthe solvent was evaporated under reduced pressure
6. customthe residue was purified by silica gel column chromatography (elution solvent:methylene chloride/methanol=40/1-20/1)

ORDレコード

ord-ff6fff21a7a444158806263321d1e9e5

出典データセット

uspto-grants-2012_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08158790B2