Triethylamine → t-butyl N-chlorothio-N-methylcarbamate

Temperatur

5 °C

To a solution of 62 g (0.6 mole) of sulfur dichloride in 200 ml of methylene chloride cooled to 0° C. under a nitrogen atmosphere was added a solution made up of 50.9 g (0.4 mole) of t-butyl N-methylcarbamate, 44.5 g (0.44 mole) of triethylamine and 100 ml of methylene chloride. The temperature was maintained at -2° to 5° C. during the addition. After stirring for one additional hour at 5° C., the mixture was filtered under a positive nitrogen atmosphere, and the filtrate was concentrated. Solid was removed by extracting the product with hexane. After filtration the hexane solution was concentrated to give 81.5 g of t-butyl N-chlorothio-N-methylcarbamate.

1. additionwas added a solution
2. temperatureThe temperature was maintained at -2° to 5° C. during the addition
3. filtrationthe mixture was filtered under a positive nitrogen atmosphere
4. concentrationthe filtrate was concentrated
5. customSolid was removed
6. extractionby extracting the product with hexane
7. filtrationAfter filtration the hexane solution
8. concentrationwas concentrated

ORD-Eintrag

ord-e53766b730974d15ada2f85fb895bd2e

Quelldatensatz

uspto-grants-1984_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04479002