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

HRID 1794687ノート

反応式

HRID 1794687 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-fee8d5246e034db2bf8e06eee28859ba
出典データセット
uspto-grants-2006_04
特許番号
US07022860B2

反応ノート

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