Carbon Disulfide → HCID 14252746, compound

Temperature

40 °C

To a mixture of 29.1 g of 3-amino-1-methylpyrazole and 45 ml of triethylamine was added dropwise 18 ml of carbon disulfide and the resulting mixture was stirred at 40° C. for 30 minutes to precipitate solids. To the reaction mixture was added ether, followed by pulverization of solids. After filtration, the thus pulverized solids were washed with ether to give 67 g of triethylamine salt of 1-methyl-3-pyrazolyldithiocarbamic acid (melting point: 79° to 82° C.) 31.8 g of the thus obtained triethylamine salt of dithiocarbamic acid and 11.7 g of triethylamine were dissolved in 150 ml of methylene chloride. To the resulting solution was added at one time 34.5 g of ferric chloride 6 hydrate dissolved in 100 ml of water, followed by vigorous stirring for 10 minutes. The reaction mixture was filtered to remove insoluble solids. The organic layer was separated and then the aqueous layer was extracted with methylene chloride. After the organic layers were combined, washed with water and dried, the solvent was distilled off under reduced pressure. To the thus obtained residue was added ether to filter the insoluble solids off and the filtrate was concentrated under reduced pressure to give 9.0 g of oil. The thus obtained oil was evaporated under reduced pressure to give 6.5 g of the desired compound. b.p.: 135° to 138° C./23 mmHg.

1. customto precipitate solids
2. additionTo the reaction mixture was added ether
3. filtrationAfter filtration
4. washthe thus pulverized solids were washed with ether

ORD record

ord-2276cabfcc5f42a6a35704acfb870a37

Source dataset

uspto-grants-1989_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04830660