Chlorosulfonic acid → 5-tert-Butyl-2-methoxybenzene-1-sulfonyl chloride

HRID 543383

反応式

HRID 543383 の反応式
[CH3:1][C:2]([C:5]1[CH:10]=[CH:9][C:8]([O:11][CH3:12])=[CH:7][CH:6]=1)([CH3:4])[CH3:3].[Cl:13][S:14](O)(=[O:16])=[O:15]>C(Cl)Cl>[CH3:4][C:2]([C:5]1[CH:10]=[C:9]([S:14]([Cl:13])(=[O:16])=[O:15])[C:8]([O:11][CH3:12])=[CH:7][CH:6]=1)([CH3:1])[CH3:3]

参加物

4

反応物 2

HCID 24638Chlorosulfonic acidHCID 94750p-tert-Butylanisole

生成物 1

HCID 132102315-tert-Butyl-2-methoxybenzene-1-sulfonyl chloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

12.3 g (0.075 mol) of 4-(1,1-dimethylethyl)anisole, dissolved in 30 ml of methylene chloride, are added dropwise, while cooling in ice, to 16.5 ml of chlorosulfonic acid dissolved in 20 ml of methylene chloride. The mixture is stirred for 40 minutes and then poured onto ice-water. The organic phase is separated off, washed with water, dried with MgSO4 and evaporated. Recrystallization from toluene/petroleum ether provides crystals of melting point: 75°-77° C.

後処理

  1. additionare added dropwise
  2. additionpoured onto ice-water
  3. customThe organic phase is separated off
  4. washwashed with water
  5. dry with materialdried with MgSO4
  6. customevaporated
  7. customRecrystallization from toluene/petroleum ether
  8. customprovides crystals of melting point: 75°-77° C.

出典と根拠

ORDレコード
ord-f9f199b4c65f4ba5ba2aa44d9e2f1c25
出典データセット
uspto-grants-1987_04
特許番号
US04661636

関連ノート

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