反应详情

温度

110 °C

A solution of 40 g of 4-chloro-6,7-dihydro-5H-cyclopenta[d]pyrmidine-1-oxide [prepared as described in step (a) above] in 1 liter of acetic anhydride was added dropwise, whilst heating at 50° C., to 1.5 liters of acetic anhydride. After the addition was complete, the solution was stirred at 110° C. for 2 hours. At the end of this time, the mixture was cooled to room temperature, and the solvent was evaporated off under reduced pressure. 400 ml of a mixture of toluene and hexane were added to the resulting residue, the mixture was stirred, and the solvent was separated by decantation; these operations were repeated a further 2 times. The decanted solvents were combined and then evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography, using chloroform as the eluent, to give 39.3 g of the title compound as a colorless oil.

1. additionAfter the addition
2. temperatureAt the end of this time, the mixture was cooled to room temperature
3. customthe solvent was evaporated off under reduced pressure
4. addition400 ml of a mixture of toluene and hexane were added to the resulting residue
5. stirringthe mixture was stirred
6. customthe solvent was separated by decantation
7. customevaporated under reduced pressure
8. customThe resulting residue was purified by silica gel column chromatography