3-Methylthiophene → 3-Methylthiophene-2-sulfonyl chloride

HRID 1730067

反応式

HRID 1730067 の反応式
[CH3:1][C:2]1[CH:6]=[CH:5][S:4][CH:3]=1.[Cl:7][S:8](O)(=[O:10])=[O:9]>C(Cl)(Cl)Cl.C(=O)(O)[O-].[Na+]>[CH3:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[S:8]([Cl:7])(=[O:10])=[O:9]

参加物

5

反応物 2

HCID 120243-MethylthiopheneHCID 24638Chlorosulfonic acid

生成物 1

HCID 134257133-Methylthiophene-2-sulfonyl chloride

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 516892Sodium Bicarbonate溶媒

反応条件

温度
25 °C

実験手順

A 49-g (0.5 mol) sample of 3-methylthiophene was added in small portions to a cooled solution (-20° C) of 128 g (1 mol) chlorosulfonic acid in 250 cc chloroform. After the addition was completed, the reaction mixture was allowed to warm to about 25° C and then heated at reflux for 30 minutes. The reaction mixture was then diluted with ice water and neutralized with aqueous sodium bicarbonate solution. The organic layer was separated, dried over magnesium sulfate and evaporated to give 30 g of 3-methyl-2-thienylsulfonyl chloride.

後処理

  1. additionAfter the addition
  2. temperatureheated
  3. temperatureat reflux for 30 minutes
  4. customThe organic layer was separated
  5. dry with materialdried over magnesium sulfate
  6. customevaporated

出典と根拠

ORDレコード
ord-daee733669fe41d397471f0f084a84c8
出典データセット
uspto-grants-1976_11
特許番号
US03991081

関連ノート

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