Reaktion #5740

Reaktionsgleichung

methanol

chlorosulfonyl isocyanate

→

white solid

Ausbeute 75.4%

Methyl(chlorosulfonyl)carbamate

Ausbeute 75.4%

Lösungsmittel

toluene

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe mixture was removed from the cooling bath
2. 2
   Temperaturcooled to 0° C.
3. 3
   workup.ADDITION65 mL ice cold hexanes was added
4. 4
   FiltrationThe white precipitate was collected by filtration
5. 5
   Waschenwashed two times with a small amount of cold hexanes
6. 6
   Sonstigedried in vacuo

Vorschrift

A solution of methanol (10.2 mL, 252 mmoles) in 15 mL toluene was added dropwise to a solution of chlorosulfonyl isocyanate (22.0 mL, 252 mmoles) in 75 mL toluene at 0° C. The mixture was removed from the cooling bath and stirred for one-half hour at room temperature, then cooled to 0° C. and 65 mL ice cold hexanes was added. The white precipitate was collected by filtration and washed two times with a small amount of cold hexanes and dried in vacuo to give 33.0 g of a white solid, mp 72°-74° C.

Quelle