反应详情

19.52 ml (0.10 mol) of N-methyl-N-trimethylsilyltrifluoroacetamide was added to a suspension of 4.20 g (0.025 mol) of 3,4-dihydroxybenzoic acid, hydrazide in 25 ml of dry acetonitrile. Stirring was continued at room temperature until a clear solution was formed (40 minutes). After evaporation in vacuo at 30°-40° C., the residue was dissolved in 25 ml of dry dichloromethane. This solution was dropped into a stirred suspension of 5.72 g (25.0 mmol) of [[[(phenylmethoxy)carbonyl]hydrazino]carbonyl]chloride at 5° C. After stirring for 1 hour at 0° C., the mixture was evaporated in vacuo and the oily residue was stirred with ether containing 4 ml of methanol until it became crystalline; yield after washing with ether and drying in vacuo: 8.77 g.

1. customwas continued at room temperature until a clear solution
2. customwas formed (40 minutes)
3. customAfter evaporation in vacuo at 30°-40° C.
4. dissolutionthe residue was dissolved in 25 ml of dry dichloromethane
5. stirringAfter stirring for 1 hour at 0° C.
6. customthe mixture was evaporated in vacuo
7. stirringthe oily residue was stirred with ether containing 4 ml of methanol until it
8. customyield
9. washafter washing with ether
10. customdrying in vacuo