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

HRID 2248903ノート

反応式

HRID 2248903 の反応式
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

参加物

4

反応物 3

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

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8930254b2c5743b782014f9bfa346773
出典データセット
uspto-grants-1991_08
特許番号
US05041453

反応ノート

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