Hydrochloric Acid → Methyl 5-hydroxy-3-methylbenzo(b)thiophene-2-carboxylate

HRID 2248903노트

반응식

HRID 2248903 반응식
Cl.[OH:2][C:3]1[CH:15]=[CH:14][C:6]2[S:7][C:8]([C:11]([OH:13])=[O:12])=[C:9]([CH3:10])[C:5]=2[CH:4]=1.[CH3:16]O>>[OH:2][C:3]1[CH:15]=[CH:14][C:6]2[S:7][C:8]([C:11]([O:13][CH3:16])=[O:12])=[C:9]([CH3:10])[C:5]=2[CH:4]=1

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 125755615-Hydroxy-3-methylbenzo[b]thiophene-2-carboxylic acid

생성물 1

HCID 19994682Methyl 5-hydroxy-3-methylbenzo(b)thiophene-2-carboxylate

실험 절차

Dry HCl gas is bubbled through a solution of 5-hydroxy-3-methylbenzo(b)thiophene-2-carboxylic acid (1.0 g, 4.81 mmol) in methanol (150 ml) for 1 hour at room temperature. The brown solution is refluxed for 2 hours and concentrated. Extraction with ether, washing with water, aqueous sodium bicarbonate, water and bring, drying (MgSO4) and concentration affords the crude product which is subjected to flash chromatography over silica gel. Elution with 33% ethyl acetate in hexane affords methyl 5-hydroxy-3-methylbenzo(b)thiophene-2-carboxylate.

후처리

  1. temperatureThe brown solution is refluxed for 2 hours
  2. concentrationconcentrated
  3. extractionExtraction with ether
  4. washwashing with water, aqueous sodium bicarbonate, water
  5. customdrying
  6. concentration(MgSO4) and concentration
  7. customaffords the crude product which
  8. washElution with 33% ethyl acetate in hexane

출처 및 근거

ORD 기록
ord-8930254b2c5743b782014f9bfa346773
출처 데이터셋
uspto-grants-1991_08
특허 번호
US05041453

반응 노트

불러오는 중…