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

HRID 9682

반응식

HRID 9682 반응식
[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]

참가 물질

3

반응물 2

HCID 887MethanolHCID 219863493-Methyl-5-[4-(trifluoromethyl)phenyl]thiophene-2-carboxylic acid2회

생성물 1

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

반응 조건

온도
30 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-39764b49df2e448c85ecf3cdf691af3a
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091237B2

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