반응 #44230

ord-99b7cf4d4099400eb317131ba24131a7

반응 방정식

Cl
HCl
CCOC(=O)c1c(Cl)c(C)c(=O)n(C)c1C(C)=O
2-acetyl-4-chloro-1,5-dimethyl-6-oxo-1,6-dihydropyridine-3-carboxylic acid ethyl ester
[Li+].[OH-]
LiOH
CC(=O)c1c(C(=O)O)c(Cl)c(C)c(=O)n1C
desired product
CC(=O)c1c(C(=O)O)c(Cl)c(C)c(=O)n1C
2-acetyl-4-chloro-1,5-dimethyl-6-oxo-1,6-dihydropyridine-3-carboxylic acid

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted with ethyl acetate
  2. 2
    건조The combined organic extracts are dried (MgSO4)
  3. 3
    농축concentrated under reduced pressure

실험 절차

To a solution of 2-acetyl-4-chloro-1,5-dimethyl-6-oxo-1,6-dihydropyridine-3-carboxylic acid ethyl ester (1.00 equivalent) in THF:water (4:1) is added 1 M aqueous LiOH solution (2.05 equivalents). After 30 minutes, the reaction mixture is acidified to pH ˜1 with 1 N HCl solution and extracted with ethyl acetate. The combined organic extracts are dried (MgSO4) and concentrated under reduced pressure to give the desired product which is used directly without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07732616B2uspto-grants-2010_06