反応 #164679

ord-e4500a20d89a4aafa3a9db98fd3661f1

反応方程式

CCOC(=O)CC(=O)CCl
Ethyl 4-chloroacetoacetate
CC(C)(C)S
2-methyl-2-propanethiol
CCN(CC)CC
triethylamine
CCOC(=O)CC(=O)CSC(C)(C)C
desired product
CCOC(=O)CC(=O)CSC(C)(C)C
4-tert-Butylsulfanyl-3-oxo-butyric acid ethyl ester

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONSilica gel was added
  2. 2
    濃縮the mixture was concentrated
  3. 3
    ろ過filtered over a plug of silica gel

実験手順

Ethyl 4-chloroacetoacetate (7.5 mL, 51.9 mmol), 2-methyl-2-propanethiol (5.6 mL, 49.7 mmol), triethylamine (10.8 mL, 77.4 mmol), and catalytic tetrabutylammonium bromide were dissolved in THF (250 mL) and stirred at room temperature overnight. Silica gel was added, and the mixture was concentrated and filtered over a plug of silica gel to obtain the desired product (B-1), which was used without further purification.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08841295B2uspto-grants-2014_09