反应详情

2.6 g of (+)-5-(o-chlorophenyl)-1,3-dihydro-3-methyl-7-nitro-2H-1,4-benzodiazepin-2-one are dissolved in 40 ml of dioxane and treated with 1.6 g of phosphorus pentasulfide and 0.7 ml of triethylamine. The mixture is then heated to reflux for 20 minutes, cooled with ice and concentrated on a rotary evaporator. The residue is treated with 10% bicarbonate solution and ethyl acetate, and the ethyl acetate phase is washed twice with 10% bicarbonate solution, dried with sodium sulfate, filtered and concentrated. The residue is purified on a 60 g silica gel column using methylene chloride and methylene chloride/ethyl acetate (20:1) for the elution and then crystallised from methylene chloride/petroleum ether. There is obtained (+)-5-(o-chlorophenyl)-1,3-dihydro-3-methyl-7-nitro-2H-1,4-benzodiazepin-2-thione which melts at 258°-260° C and which exhibits a rotation of [α]25D =+160,6° (in methylene chloride, 1%).

1. temperatureThe mixture is then heated
2. temperatureto reflux for 20 minutes
3. temperaturecooled with ice
4. concentrationconcentrated on a rotary evaporator
5. additionThe residue is treated with 10% bicarbonate solution and ethyl acetate
6. washthe ethyl acetate phase is washed twice with 10% bicarbonate solution
7. dry with materialdried with sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated
10. customThe residue is purified on a 60 g silica gel column
11. washfor the elution
12. customcrystallised from methylene chloride/petroleum ether