Methanol → Methyl chlorosulfonylcarbamate

HRID 5644

Reaktionsgleichung

Reaktionsgleichung von HRID 5644
[CH3:1][OH:2].[Cl:3][S:4]([N:7]=[C:8]=[O:9])(=[O:6])=[O:5]>C1(C)C=CC=CC=1>[CH3:1][O:2][C:8](=[O:9])[NH:7][S:4]([Cl:3])(=[O:6])=[O:5]

Komponenten

4

Edukt 2

HCID 887MethanolHCID 70918Chlorosulfonyl isocyanate

Produkt 1

HCID 10702364Methyl chlorosulfonylcarbamateAusbeute 75,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel2×

Versuchsvorschrift

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.

Aufarbeitung

  1. customThe mixture was removed from the cooling bath
  2. temperaturecooled to 0° C.
  3. addition65 mL ice cold hexanes was added
  4. filtrationThe white precipitate was collected by filtration
  5. washwashed two times with a small amount of cold hexanes
  6. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-5b876d1b98bf447b958335604e70efcd
Quelldatensatz
uspto-grants-1993_09
Patentnummer
US05245068

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