反应详情

A mixture of 50 mL of ethanol, 1 mL of acetic acid and 1.3 g of the 3-[(5-amino-2-chloro-pyrimidin-4-yl)-butyl-amino]-propionic acid tert-butyl ester (V-44), prepared in the previous step, was heated at reflux overnight, and then concentrated under reduced pressure. The residue was taken up in dichloromethane and washed successively with 10% sodium bicarbonate solution, water and then dried over anhydrous sodium sulfate. The mixture was filtered and then concentrated under reduced pressure. Trituration of the residue with ether, provided 0.90 g of 9-butyl-2-chloro-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one (VI-44).

1. customprepared in the previous step
2. temperaturewas heated
3. temperatureat reflux overnight
4. concentrationconcentrated under reduced pressure
5. washwashed successively with 10% sodium bicarbonate solution, water
6. dry with materialdried over anhydrous sodium sulfate
7. filtrationThe mixture was filtered
8. concentrationconcentrated under reduced pressure