反应详情

A mixture of 0.2224 g (0.00068 mole) of 1-{[(5-amino-2-chloro-pyrimidin-4-yl)-cyclopentyl-amino]-methyl}-cyclopropanecarboxylic acid methyl ester (V-53), 12 mL of ethanol and 0.3 mL of acetic acid was heated at reflux for 18 hours, and then concentrated under reduced pressure. The residue was dissolved in 100 mL of ethyl acetate and washed successively twice with 15 mL of aqueous sodium bicarbonate, twice with 15 mL of brine, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to give 0.195 g of 2-chloro-9-cyclopentyl-8,9-dihydro-spiro[5H-pyrimido[4,5-b][1,4]diazepine-7,1′-cyclopropan]-6(7H)-one (VI-53), as a light yellow solid.

1. temperaturewas heated
2. temperatureat reflux for 18 hours
3. concentrationconcentrated under reduced pressure
4. dissolutionThe residue was dissolved in 100 mL of ethyl acetate
5. washwashed successively twice with 15 mL of aqueous sodium bicarbonate, twice with 15 mL of brine
6. dry with materialdried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure