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Methanol → Methyl 5-ethoxy-6-hydroxybenzo[b]thiophene-2-carboxylate

HRID 1583578
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HRID 1583578 반응식
[CH2:1]([O:3][C:4]1[C:5]([OH:16])=[CH:6][C:7]2[S:11][C:10]([C:12]([OH:14])=[O:13])=[CH:9][C:8]=2[CH:15]=1)[CH3:2].[CH3:17]O.S(=O)(=O)(O)O>C(Cl)Cl.C(OCC)(=O)C>[CH2:1]([O:3][C:4]1[C:5]([OH:16])=[CH:6][C:7]2[S:11][C:10]([C:12]([O:14][CH3:17])=[O:13])=[CH:9][C:8]=2[CH:15]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 20259233HCID 20259233, 화합물

생성물 1

HCID 20259234Methyl 5-ethoxy-6-hydroxybenzo[b]thiophene-2-carboxylate

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

A solution of 0.71 g. of 5 -ethoxy-6-hydroxybenzothiophene-2-carboxylic acid, 0.29 g. of methanol, and a catalytic amount of sulfuric acid in methylene chloride was heated to reflux for 48 hours. The solution was diluted with ethyl acetate and was washed first with a 10% aqueous sodium bicarbonate solution and then with water. The organic solution was dried over sodium sulfate and evaporated to dryness providing the desired ester intermediate which was used without further purification.

후처리

  1. temperatureto reflux for 48 hours
  2. washwas washed first with a 10% aqueous sodium bicarbonate solution
  3. dry with materialThe organic solution was dried over sodium sulfate
  4. customevaporated to dryness

출처 및 근거

ORD 기록
ord-418b46f9bcd943b7a73b4bda3a33152e
출처 데이터셋
uspto-grants-1985_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04552891

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