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Water → ethyl (Z)-2-ethoxy-3-{3'-[methyl(4-nitrophenoxycarbonyl)amino]biphenyl-4-yl}acrylate

HRID 390678
ノート
印刷プレビュー

反応式

HRID 390678 の反応式
Cl[C:2]([O:4][C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][CH:6]=1)=[O:3].C(NCC)C.[CH2:19]([O:21]/[C:22](=[CH:28]\[C:29]1[CH:34]=[CH:33][C:32]([C:35]2[CH:40]=[CH:39][CH:38]=[C:37]([NH:41][CH3:42])[CH:36]=2)=[CH:31][CH:30]=1)/[C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH3:20].O>ClCCl>[CH2:19]([O:21]/[C:22](=[CH:28]\[C:29]1[CH:34]=[CH:33][C:32]([C:35]2[CH:40]=[CH:39][CH:38]=[C:37]([N:41]([CH3:42])[C:2]([O:4][C:5]3[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][CH:6]=3)=[O:3])[CH:36]=2)=[CH:31][CH:30]=1)/[C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH3:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8021DiethylamineHCID 821294-Nitrophenyl chloroformateHCID 86626079ethyl (Z)-2-ethoxy-3-(3'-methylaminobiphenyl-4-yl)acrylate

生成物 1

HCID 86626081ethyl (Z)-2-ethoxy-3-{3'-[methyl(4-nitrophenoxycarbonyl)amino]biphenyl-4-yl}acrylate収率 126.2%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

0.63 g (3.1 mmol) of 4-nitrophenyl chloroformate and then 0.54 mL (3.1 mmol) of diethylamine are added to a solution of 0.68 g (2.1 mmol) of ethyl (Z)-2-ethoxy-3-(3′-methylaminobiphenyl-4-yl)acrylate in 15 mL of dichloromethane. The reaction mixture is stirred for 1 hour 30 minutes at room temperature. The reaction is worked up by addition of 10 mL of water and then extracted with dichloromethane. The organic phases are combined and then dried over magnesium sulfate. The solvents are evaporated off. 1.3 g (100%) of ethyl (Z)-2-ethoxy-3-{3′-[methyl-(4-nitrophenoxycarbonyl)amino]biphenyl-4-yl}acrylate are obtained in the form of a yellow oil.

後処理

  1. extractionextracted with dichloromethane
  2. dry with materialdried over magnesium sulfate
  3. customThe solvents are evaporated off

出典と根拠

ORDレコード
ord-fa17fca0c2414bec984c3b6134d3eb22
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08383652B2

反応ノート

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