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

HRID 543383

Reaktionsgleichung

Reaktionsgleichung von HRID 543383
[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]

Komponenten

4

Edukt 2

HCID 24638Chlorosulfonic acidHCID 94750p-tert-Butylanisole

Produkt 1

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

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

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.

Aufarbeitung

  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.

Quellen und Nachweise

ORD-Eintrag
ord-f9f199b4c65f4ba5ba2aa44d9e2f1c25
Quelldatensatz
uspto-grants-1987_04
Patentnummer
US04661636

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