Carbon Tetrachloride → HCID 54314601, compound

A mixture of isopropylhydrazine (7.42 g, 0.1 mole), potassium carbonate (20.73 g, 0.15 mole) and triethylbenzyl ammonium chloride (0.3 g, 0.0013 mole was stirred vigorously at reflux with dichloromethane (100 ml) and carbon tetrachloride (60 ml) for 30 minutes. A solution of dimethylchlorothiophosphate (16.6 g, 0.1 mole) in dichloromethane (20 ml) was then added dropwise to this refluxing mixture and the mixture stirred and refluxed for an additional 20 hours. The mixture was then filtered and the filtrate dried over anhydrous magnesium sulfate. The dried filtrate, then was evaporated down to a viscous oil which was subjected to high vacuum for 2 or 3 hours to yield 6.5 g of a thick yellow oil, nD25° =1.5132, identified as the product by NMR, IR and mass spectroscopy.

1. stirringthe mixture stirred
2. temperaturerefluxed for an additional 20 hours
3. filtrationThe mixture was then filtered
4. dry with materialthe filtrate dried over anhydrous magnesium sulfate
5. customThe dried filtrate, then was evaporated down to a viscous oil which
6. customwas subjected to high vacuum for 2 or 3 hours

ORD record

ord-c97388c0abd74062b34a7bc5cc51d171

Source dataset

uspto-grants-1980_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04203932