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Ethanol → Ethyl-5-(4-chlorophenyl)-4-methyl-3-(4-sulfamoylphenyl)thiophene-2-carboxylate

HRID 1053247
ノート
印刷プレビュー

反応式

HRID 1053247 の反応式
[CH3:1][O:2][C:3]([C:5]1[S:6][C:7]([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][CH:13]=2)=[C:8]([CH3:11])[C:9]=1Br)=[O:4].[CH2:19](O)C.[NH2:22][S:23]([C:26]1[CH:31]=[CH:30][C:29](B(O)O)=[CH:28][CH:27]=1)(=[O:25])=[O:24].C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH2:1]([O:2][C:3]([C:5]1[S:6][C:7]([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][CH:13]=2)=[C:8]([CH3:11])[C:9]=1[C:29]1[CH:30]=[CH:31][C:26]([S:23](=[O:25])(=[O:24])[NH2:22])=[CH:27][CH:28]=1)=[O:4])[CH3:19]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 702EthanolHCID 11430Potassium CarbonateHCID 223919774-(Aminosulphonyl)benzeneboronic acidHCID 68285497Methyl 3-bromo-5-(4-chlorophenyl)-4-methylthiophene-2-carboxylate2 回

生成物 1

HCID 68285835Ethyl-5-(4-chlorophenyl)-4-methyl-3-(4-sulfamoylphenyl)thiophene-2-carboxylate収率 48%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒
HCID 1140Toluene溶媒

反応条件

温度
25 °C

実験手順

To a solution of methyl-3-bromo-5-(4-chlorophenyl)-4-methylthiophene-2-carboxylate (compound 1a, 2.2 g, 6.3 mmol) in a mixture of toluene: ethanol (10:30 ml) were added 4-aminosulfonylbenzene boronic acid (prepared according to the procedure given in EP 1012142, 1.28 g, 6.3 mmol) and potassium carbonate (1.76 g, 12.7 mmol) at 25° C. in a sealed tube and nitrogen gas was bubbled through the reaction mixture for 15 minutes. To this was added tetrakis(triphenylphosphine)palladium(0) (0.370 g, 0.318 mmol) under nitrogen and the reaction mixture was heated at about 95-about 100° C. for 18 hr under stirring. The progress of the reaction was monitored by TLC. The reaction mixture was cooled to 25° C. and filtered through celite. The filtrate was concentrated under reduced pressure to obtain a crude product, which was purified by column chromatography over silica gel (100-200 mesh) using 40% ethyl acetate in hexanes as an eluent to obtain the title compound (1.3 g, 48%).

後処理

  1. customprepared
  2. customat 25° C.
  3. customnitrogen gas was bubbled through the reaction mixture for 15 minutes
  4. temperaturethe reaction mixture was heated at about 95-about 100° C. for 18 hr
  5. filtrationfiltered through celite
  6. concentrationThe filtrate was concentrated under reduced pressure
  7. customto obtain a crude product, which
  8. customwas purified by column chromatography over silica gel (100-200 mesh)

出典と根拠

ORDレコード
ord-6c91b5b23c10491cb24586a1867da09e
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09393247B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート