Hydrochloric Acid → Carbonic acid 4-nitro-phenyl ester (R)-1-phenyl-ethyl ester

温度

0 °C

A mixture of (R)-1-phenyl-ethanol (60.6 g, 0.496 mol), pyridine (42.5 mL, 0.526 mol) and 2-methyl-tetrahydrofuran (600 mL) was cooled to 0° C. and p-nitrophenyl chloroformate (100 g, 0.496 mol) was added over 15 min keeping the internal temperature below 5° C. The reaction mixture was warmed to room temperature and stirred for 2 h. To the reaction mixture was added 1.0 M HCl in water (300 mL). Layers were separated. The organic layer was washed with 1N HCl (300 mL) and brine (300 mL), filtered, concentrated to dryness by rotary evaporation, and dried under vacuum to give the title compound (140 g) as a clear yellow oil.

1. customthe internal temperature below 5° C
2. temperatureThe reaction mixture was warmed to room temperature
3. customLayers were separated
4. washThe organic layer was washed with 1N HCl (300 mL) and brine (300 mL)
5. filtrationfiltered
6. concentrationconcentrated to dryness by rotary evaporation
7. customdried under vacuum

ORDレコード

ord-d7f9b1ad62e54ccaa2ada1d9c08a0333

出典データセット

uspto-grants-2012_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08106232B2