Reaktion #5741

ord-0b945865b6ed43e89b1d0e52682f9023

Reaktionsgleichung

CCCCCCCCCCCCO
n-dodecyl alcohol
O=C=NS(=O)(=O)Cl
chlorosulfonyl isocyanate
CCCCCCCCCCCCOC(=O)NS(=O)(=O)Cl
white solid
Ausbeute 101.6%
CCCCCCCCCCCCOC(=O)NS(=O)(=O)Cl
Dodecyl(chlorosulfonyl)carbamate
Ausbeute 101.6%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenconcentrated in vacuo
  2. 2
    SonstigeThe residue was triturated with cold hexanes
  3. 3
    Sonstigeto give a white solid
  4. 4
    Filtrationcollected by filtration

Vorschrift

A solution of n-dodecyl alcohol (10.7 g, 57.4 mmoles) in 100 mL Et2O was added dropwise to a solution of chlorosulfonyl isocyanate (5.0 mL, 57.4 mmoles) in 100 mL Et2O at ~15° C. under an atmosphere of N2. The resulting mixture was stirred for 2 hours and concentrated in vacuo. The residue was triturated with cold hexanes to give a white solid and collected by filtration to give 19.12 g of a white solid, mp 62°-63° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05245068uspto-grants-1993_09