Chlorosulfonic acid → 7-Nitrodibenzo[b,d]furan-2-sulfonyl chloride

HRID 636932Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 636932
[N+:1]([C:4]1[CH:5]=[CH:6][C:7]2[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[O:9][C:8]=2[CH:16]=1)([O-:3])=[O:2].[Cl:17][S:18](O)(=[O:20])=[O:19]>ClCCl>[N+:1]([C:4]1[CH:5]=[CH:6][C:7]2[C:11]3[CH:12]=[C:13]([S:18]([Cl:17])(=[O:20])=[O:19])[CH:14]=[CH:15][C:10]=3[O:9][C:8]=2[CH:16]=1)([O-:3])=[O:2]

Komponenten

4

Edukt 2

HCID 24638Chlorosulfonic acidHCID 728973-Nitrodibenzofuran

Produkt 1

HCID 109030227-Nitrodibenzo[b,d]furan-2-sulfonyl chloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a stirred solution of 100 mg of 3-nitrodibenzofuran in 1.7 mL of dichloromethane at −20° C. under a nitrogen atmosphere was added 0.44 mL chlorosulfonic acid in small portions. The reaction mixture was allowed to slowly warm to room temperature and stirred for 66 hours at room temperature. The reaction mixture was poured into ice-cold water, extracted four times with dichloromethane, dried (magnesium sulfate) and concentrated. Purification on silica gel (dichloromethane) yielded 129 mg of 50a: rf=0.73.

Aufarbeitung

  1. additionThe reaction mixture was poured into ice-cold water
  2. extractionextracted four times with dichloromethane
  3. dry with materialdried (magnesium sulfate)
  4. concentrationconcentrated
  5. customPurification on silica gel (dichloromethane)

Quellen und Nachweise

ORD-Eintrag
ord-d668e9cb891f43bd86cb6b09ecb2adbd
Quelldatensatz
uspto-grants-2001_02
Patentnummer
US06194409B1

Notizen zur Reaktion

Wird geladen…