Methanol → Methyl chlorosulfonylcarbamate

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.

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

ORDレコード

ord-5b876d1b98bf447b958335604e70efcd

出典データセット

uspto-grants-1993_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05245068