Carbon Tetrachloride → HCID 15616511, Verbindung

HRID 622305Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 622305
O[CH2:2][CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10]([NH:13][C:14]([CH3:17])([CH3:16])[CH3:15])(=[O:12])=[O:11].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:38]>>[Cl:38][CH2:2][CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10]([NH:13][C:14]([CH3:17])([CH3:16])[CH3:15])(=[O:12])=[O:11]

Komponenten

4

Edukt 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 138229722-(2-hydroxyethyl)-N-(1,1-dimethylethyl)benzenesulfonamide

Produkt 1

HCID 15616511HCID 15616511, Verbindung

Versuchsvorschrift

A solution of 32.5 g of the alcohol from Example 1 and 32.5 g triphenylphosphine in 244 ml of carbon tetrachloride was stirred at room temperature and under an atmosphere of nitrogen for 72 hours. Excess carbon tetrachloride was removed in vacuo to give 83 g of a crude yellow oil. Purification by silica gel chromatography (hexanes-20% ethyl acetate) afforded a colorless viscous oil which crystallized on standing. The product was isolated by trituration with hexanes, filtration, and drying. The yield of pure 2-(2-chloroethyl)-N-(1,1-dimethylethyl)benzenesulfonamide, m.p. 64°-65° C., was 15.9 g.

Aufarbeitung

  1. customExcess carbon tetrachloride was removed in vacuo
  2. customto give 83 g of a crude yellow oil
  3. customPurification by silica gel chromatography (hexanes-20% ethyl acetate)
  4. customafforded a colorless viscous oil which
  5. customcrystallized
  6. customThe product was isolated by trituration with hexanes, filtration
  7. customdrying

Quellen und Nachweise

ORD-Eintrag
ord-7a5f12008c21451da6fd0c1eaa6b6369
Quelldatensatz
uspto-grants-1988_09
Patentnummer
US04770690

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