Triethylamine → Ethyl 4-(3,4-Dimethoxyphenyl)-4-oxo-2-butynoate

HRID 1794687노트

반응식

HRID 1794687 반응식
Br[CH:2]([CH:8](Br)[C:9]([C:11]1[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[C:13]([O:19][CH3:20])[CH:12]=1)=[O:10])[C:3]([O:5][CH2:6][CH3:7])=[O:4].C(N(CC)CC)C.COC1C=C(C(=O)C#CC(OC)=O)C=CC=1OC>C(Cl)Cl>[CH3:20][O:19][C:13]1[CH:12]=[C:11]([C:9](=[O:10])[C:8]#[C:2][C:3]([O:5][CH2:6][CH3:7])=[O:4])[CH:16]=[CH:15][C:14]=1[O:17][CH3:18]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 22222579Methyl 4-(3,4-dimethoxyphenyl)-4-oxo-2-butynoateHCID 22222634Ethyl 2,3-dibromo-4-(3,4-dimethoxyphenyl)-4-oxobutanoate

생성물 1

HCID 22222587Ethyl 4-(3,4-Dimethoxyphenyl)-4-oxo-2-butynoate수율 82%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of ethyl 2,3-dibromo-4-(3,4-dimethoxyphenyl)-4-oxobutanoate (4.76 g, 11.2 mmol), prepared above, in methylene chloride (20 ml) and a solution of triethylamine (4 g) in methylene chloride (5 ml) were subjected to reaction and treatment in the same manner as described above in connection with Intermediate 1. The crude product was purified by column chromatography on silica gel (hexane/ethyl acetate) to give the title compound (2.4 g, 82%) as a yellow crystal.

후처리

  1. customThe crude product was purified by column chromatography on silica gel (hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-fee8d5246e034db2bf8e06eee28859ba
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07022860B2

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