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

HRID 1583363ノート

反応式

HRID 1583363 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

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

実験手順

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°).

後処理

  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

出典と根拠

ORDレコード
ord-4843a1c6f8eb4b99a3a208ceab57183d
出典データセット
uspto-grants-1985_11
特許番号
US04551468

反応ノート

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