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

HRID 543383노트

반응식

HRID 543383 반응식
[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]

참가 물질

4

반응물 2

HCID 24638Chlorosulfonic acidHCID 94750p-tert-Butylanisole

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-f9f199b4c65f4ba5ba2aa44d9e2f1c25
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04661636

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