反应详情

To a solution of 4.55 g. of 85% potassium hydroxide in 93 mml. of methanol cooled to 5°, was added 17.0 g. of 5-bromo-1-cyclopropylmethyl-5,6-dihydrocytosine. The mixture was stirred and allowed to warm spontaneously. When the initial reaction, which had warmed the mixture to 30°, subsided, the mixture was refluxed for 5 minutes and allowed to cool and stand at room temperature overnight. The suspension was evaporated under reduced pressure on a water bath at 86°. The residue was triturated was 300 ml. of water on a steam bath and chilled in ice before filtering. The resulting 1-cyclopropylmethylcytosine was washed with cold water and dried in a vacuum desiccator over potassium hydroxide; yield, 9.50 g., m.p. 264°-266°. A sample for analysis was recrystallized from ethanol; m.p. 265°-267°.

1. additionwas added 17.0 g
2. temperatureto warm spontaneously
3. customWhen the initial reaction, which
4. temperaturehad warmed the mixture to 30°
5. temperaturethe mixture was refluxed for 5 minutes
6. temperatureto cool
7. customThe suspension was evaporated under reduced pressure on a water bath at 86°
8. customThe residue was triturated
9. temperatureof water on a steam bath and chilled in ice
10. filtrationbefore filtering
11. washThe resulting 1-cyclopropylmethylcytosine was washed with cold water
12. dry with materialdried in a vacuum desiccator over potassium hydroxide
13. customyield
14. customA sample for analysis was recrystallized from ethanol