Methanol → Methyl 5-chlorothiophene-2-carboxylate

HRID 1961003노트

반응식

HRID 1961003 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-carboxylate

반응 조건

온도
50 °C

실험 절차

To a solution of 5-chloro-2-thiophenecarboxylic acid (2.0 g, 12.3 mmol) in dry MeOH (75 mL) was added H2SO4 (1 mL). The reaction mixture was heated to 50° C. for 20 h and was then concentrated under vacuum. The residue was dissolved in DCM and washed several times with saturated NaHCO3 solution. The organic fraction was dried (Na2SO4), concentrated under vacuum and used directly without further purification 21.3 g, quant.): LC-MS (ES) m/z=177 (M+H)+.

후처리

  1. concentrationwas then concentrated under vacuum
  2. dissolutionThe residue was dissolved in DCM
  3. washwashed several times with saturated NaHCO3 solution
  4. dry with materialThe organic fraction was dried (Na2SO4)
  5. concentrationconcentrated under vacuum
  6. customused directly without further purification 21.3 g

출처 및 근거

ORD 기록
ord-8a870296d64f40c583b1d74acc462f10
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08410158B2

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