反应详情

A mixture of 0.0203 g (0.000066 mole) of 2-chloro-9-cyclopentyl-5,7,7-trimethyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one (VII-38), 0.0207 g (0.000077 mole) of N-(1-methyl-piperidin-4-yl)-4-nitro-benzenesulfonamide, 0.6 mL of ethanol, 2.4 mL of water and 2 drops of hydrochloric acid was heated at reflux for 17 hrs. The mixture was taken up in 50 mL of ethyl acetate and washed successively twice with 7 mL of 1M sodium hydroxide, twice with 7 mL of water and 7 mL of brine. The organic layer was concentrated under reduced pressure and the residue purified by silica gel chromatography, elution with dichloromethane-methanol 95:5-80:20) gave 0.0151 g of 4-(9-cyclopentyl-5,7,7-trimethyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-N-(1-methyl-piperidin-4-yl)-benzenesulfonamide (I-64) as an off-white solid.

1. temperaturewas heated
2. temperatureat reflux for 17 hrs
3. washwashed successively twice with 7 mL of 1M sodium hydroxide, twice with 7 mL of water and 7 mL of brine
4. concentrationThe organic layer was concentrated under reduced pressure
5. customthe residue purified by silica gel chromatography, elution with dichloromethane-methanol 95:5-80:20)