Ethanol → Ethyl 5-bromo-3-methyl-1-benzothiophene-2-carboxylate

HRID 1583363노트

반응식

HRID 1583363 반응식
[Br:1][C:2]1[CH:14]=[CH:13][C:5]2[S:6][C:7]([C:10]([OH:12])=[O:11])=[C:8]([CH3:9])[C:4]=2[CH:3]=1.S(=O)(=O)(O)O.[CH2:20](O)[CH3:21]>>[CH2:20]([O:11][C:10]([C:7]1[S:6][C:5]2[CH:13]=[CH:14][C:2]([Br:1])=[CH:3][C:4]=2[C:8]=1[CH3:9])=[O:12])[CH3:21]

참가 물질

4

반응물 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 202609195-Bromo-3-methyl-1-benzothiophene-2-carboxylic acid

생성물 1

HCID 54272974Ethyl 5-bromo-3-methyl-1-benzothiophene-2-carboxylate

실험 절차

A mixture of 5-bromo-3-methylbenzo[b]thiophene-2-carboxylic acid (5.80 g.), ethanol (500 ml.) and concentrated sulphuric acid (2 ml.) was heated under reflux for 48 hours, and then evaporated. Dilute aqueous ammonia solution was added and the solid was filtered off, washed well with water and dried to give 5-bromo-3-methylbenzo[b]thiophene-2-carboxylic acid ethyl ester (5.70 g.), m.p. 87°-88° C., raised to 88°-89° on crystallization from petrol (b.p. 80°-100°).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 48 hours
  3. customevaporated
  4. additionDilute aqueous ammonia solution was added
  5. filtrationthe solid was filtered off
  6. washwashed well with water
  7. customdried

출처 및 근거

ORD 기록
ord-4843a1c6f8eb4b99a3a208ceab57183d
출처 데이터셋
uspto-grants-1985_11
특허 번호
US04551468

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