反应详情

To a solution of 0.37 g (0.001 mole) of (rac)-2-{[(2-chloro-5-nitro-pyrimidin-4-yl)-cyclopentyl-amino]-methyl}-butanoic acid ethyl ester in 5 mL of ethanol was added 0.562 g (0.0025 mole) of stannous chloride dihydrate and 0.1 mL of hydrochloric acid. The mixture was heated to 60 degrees for 2 hrs. The solvent was evaporated under reduced pressure. The residue was taken up in 20 mL of water and extracted with three times with 20 mL of ethyl acetate. The combined organic layers were dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. Purification by silica gel chromatography, eluting with dichloromethane-methanol (100:0-95:5) gave 0.155 g of (rac)-2-chloro-9-cyclopentyl-7-ethyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one (VI-12) as a white solid.

1. temperatureThe mixture was heated to 60 degrees for 2 hrs
2. customThe solvent was evaporated under reduced pressure
3. extractionextracted with three times with 20 mL of ethyl acetate
4. dry with materialThe combined organic layers were dried over anhydrous magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customPurification by silica gel chromatography
8. washeluting with dichloromethane-methanol (100:0-95:5)