反应详情

温度

60 °C

A mixture of 0.14 g of α-chloro-N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]benzeneacetamide, 0.47 g of 2-dimethylaminoethanethiol hydrochloride in 2 ml of methyl alcohol, 0.30 g of triethylamine and 3 ml of 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone is heated at 60° C. for 48 hours. The methyl alcohol is evaporated and the residue diluted with water. The resulting suspension is filtered and the precipitate washed with water. The solid is dissolved in ethyl acetate and washed with saturated NaHCO3, brine and dried with Na2SO4. The mixture is filtered and the filtrate evaporated in vacuo to a residue which is stirred with ether-hexane to give 0.15 g of beige solid. MS(CI): 525(M+H).

1. customThe methyl alcohol is evaporated
2. additionthe residue diluted with water
3. filtrationThe resulting suspension is filtered
4. washthe precipitate washed with water
5. dissolutionThe solid is dissolved in ethyl acetate
6. washwashed with saturated NaHCO3, brine
7. dry with materialdried with Na2SO4
8. filtrationThe mixture is filtered
9. customthe filtrate evaporated in vacuo to a residue which