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

HRID 1293558노트

반응식

HRID 1293558 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-aed5be7e4180485e9bf3dfe6c377ea45
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07238812B2

반응 노트

불러오는 중…