Chlorosulfonic acid → 5-Bromo-2,3-dihydro-2-methyl-7-benzo[b]furanylsulfochloride

HRID 979734Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 979734
[Cl:1][S:2]([OH:5])(=[O:4])=[O:3].[Br:6][C:7]1[CH:16]=[CH:15][C:10]2[O:11][CH:12]([CH3:14])[CH2:13][C:9]=2[CH:8]=1>C(Cl)(Cl)Cl>[Br:6][C:7]1[CH:16]=[C:15]([O:3][S:2]([Cl:1])(=[O:5])=[O:4])[C:10]2[O:11][CH:12]([CH3:14])[CH2:13][C:9]=2[CH:8]=1

Komponenten

4

Edukt 2

HCID 24638Chlorosulfonic acidHCID 133016015-Bromo-2-methyl-2,3-dihydro-1-benzofuran

Produkt 1

HCID 867411765-Bromo-2,3-dihydro-2-methyl-7-benzo[b]furanylsulfochlorideAusbeute 65 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

470 g (4.03 moles) of chlorosulfonic acid are added dropwise over 20 minutes at -7° C. to a solution of 106 g (0.5 mole) of 5-bromo-2,3-dihydro-2-methylbenzo[b]furan in 300 ml of chloroform, and the mixture is then stirred for a further 15 minutes at 20°-25° C. The reaction mixture is taken up in ice/water, the organic phase is separated, and aqueous phase is extracted with two 500 ml portions of chloroform. The combined organic phases are washed with two 250 ml portions of water, dried over sodium sulfate, and concentrated, affording 101 g (65% of theory) of 5-bromo-2,3-dihydro-2-methyl-7-benzo[b]furanylsulfochloride.

Aufarbeitung

  1. customthe organic phase is separated
  2. extractionaqueous phase is extracted with two 500 ml portions of chloroform
  3. washThe combined organic phases are washed with two 250 ml portions of water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-4cb0146883cb465d958a1de54e18d073
Quelldatensatz
uspto-grants-1987_01
Patentnummer
US04634465

Notizen zur Reaktion

Wird geladen…