Methanol → Methyl 3-methyl-5-[4-(trifluoromethyl)phenyl]thiophene-2-carboxylate

HRID 9682

反応式

HRID 9682 の反応式
[CH3:1][C:2]1[CH:6]=[C:5]([C:7]2[CH:12]=[CH:11][C:10]([C:13]([F:16])([F:15])[F:14])=[CH:9][CH:8]=2)[S:4][C:3]=1[C:17]([OH:19])=[O:18].[CH3:20]O>>[CH3:1][C:2]1[CH:6]=[C:5]([C:7]2[CH:8]=[CH:9][C:10]([C:13]([F:14])([F:15])[F:16])=[CH:11][CH:12]=2)[S:4][C:3]=1[C:17]([O:19][CH3:20])=[O:18]

参加物

3

反応物 2

HCID 887MethanolHCID 219863493-Methyl-5-[4-(trifluoromethyl)phenyl]thiophene-2-carboxylic acid2 回

生成物 1

HCID 21986442Methyl 3-methyl-5-[4-(trifluoromethyl)phenyl]thiophene-2-carboxylate

反応条件

温度
30 °C

実験手順

A mixture of 3-methyl-5[4-(trifluoromethyl)phenyl]thiophene-2-carboxylic acid (intermediate 130, 8.1 g) in methanol (300 ml) was heated at 30° C. and hydrogen chloride gas bubbled through the mixture. The reaction mixture was then stirred at reflux for 21 hours; cooled and treated with further hydrogen chloride gas. The reaction mixture was stirred at reflux for a further 6 hours, cooled and concentrated. The resulting precipitate was filtered and washed with cyclohexane to give the title compound as a solid.

後処理

  1. customhydrogen chloride gas bubbled through the mixture
  2. temperatureat reflux for 21 hours
  3. temperaturecooled
  4. additiontreated with further hydrogen chloride gas
  5. stirringThe reaction mixture was stirred
  6. temperatureat reflux for a further 6 hours
  7. temperaturecooled
  8. concentrationconcentrated
  9. filtrationThe resulting precipitate was filtered
  10. washwashed with cyclohexane

出典と根拠

ORDレコード
ord-39764b49df2e448c85ecf3cdf691af3a
出典データセット
uspto-grants-2006_08
特許番号
US07091237B2

関連ノート

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