Methanol → Methyl 5-chlorothiophene-2-carboxylate

HRID 1961063노트

반응식

HRID 1961063 반응식
[Cl:1][C:2]1[S:6][C:5]([C:7]([OH:9])=[O:8])=[CH:4][CH:3]=1.OS(O)(=O)=O.[CH3:15]O>>[Cl:1][C:2]1[S:6][C:5]([C:7]([O:9][CH3:15])=[O:8])=[CH:4][CH:3]=1

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 950485-Chloro-2-thiophenecarboxylic acid

생성물 1

HCID 589473Methyl 5-chlorothiophene-2-carboxylate수율 99%

반응 조건

온도
55 °C

실험 절차

To a solution of 5-chloro-2-thiophenecarboxylic acid (20 g, 123 mmoles) in MeOH (200 mL) was added conc. H2SO4 (5 mL). After heating to 55° C. for 12 h, the reaction solution was concentrated and diluted with DCM (250 mL). The DCM solution was washed with aqueous NaHCO3, then H2O and dried over Na2SO4. Concentration under vacuum gave the title compound as a yellow oil (21.5 g, 99%): LCMS (ES) m/z 178 (M+H)+.

후처리

  1. concentrationthe reaction solution was concentrated
  2. additiondiluted with DCM (250 mL)
  3. washThe DCM solution was washed with aqueous NaHCO3
  4. dry with materialH2O and dried over Na2SO4
  5. concentrationConcentration under vacuum

출처 및 근거

ORD 기록
ord-21e4e8b847824c68b0d3a9e48404827d
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08410158B2

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