Ethyl 4-chloroacetoacetate → Butanoic acid, 4-chloro-3-hydroxy-, ethyl ester

Temperatur

100 °C

In a 200 ml-volume stainless steel-made autoclave whose atmosphere had been replaced with nitrogen were charged 8.23 g (50 mmoles) of ethyl 4-chloroacetoacetate and 20 ml of ethanol. To the mixture was added 84 mg (0.05 mmole) of Ru2Cl4 ((-)-BINAP)2 (C2H5)3N, and the mixture was heated to 100° C. When the temperature reached 100° C., 100 kg/cm2 of hydrogen was introduced into the autoclave, and the mixture was stirred under heating. After cooling to room temperature, the reaction mixture was taken out, and the ethanol was removed by distillation. Distillation of the residue gave 8.07 g (97) of ethyl 4-chloro-3-hydroxybutyrate having a boiling point of 74°-75° C./l mmHg).

1. customreached 100° C.
2. temperatureunder heating
3. temperatureAfter cooling to room temperature
4. customthe ethanol was removed by distillation
5. distillationDistillation of the residue

ORD-Eintrag

ord-1a18d63915d444e2a7705bff2e567dc3

Quelldatensatz

uspto-grants-1990_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04895979