反应详情

To a slurry of 2.25 grams (.025 moles) of carbohydrazide in 30 ml of methanol stirred by a magnetic stirrer in a 50 ml erlenmeyer flask was added 11.3 grams (.05 moles) of 1-t-butylazo-1-isothiocyanatocyclohexane (from Example I). The reaction was stirred overnight, during which time complete solution was obtained. The next morning the solution was poured into 200 ml water and the product extracted with methylene chloride. The methylene chloride extract was washed with water, dried over anhydrous Na2SO4, filtered and the methylene chloride evaporated under reduced pressure to leave 11.9 grams (87.5% crude yield) of a yellow viscous liquid that slowly crystallized.

1. customwas obtained
2. extractionthe product extracted with methylene chloride
3. extractionThe methylene chloride extract
4. washwas washed with water
5. dry with materialdried over anhydrous Na2SO4
6. filtrationfiltered
7. customthe methylene chloride evaporated under reduced pressure
8. customto leave 11.9 grams (87.5% crude yield) of a yellow viscous liquid that
9. customslowly crystallized