反应详情

To a solution of 125 ml. of absolute ethanol saturated with ammonia was added 2.0 g. ammonium chloride and 25.7 g. (0.124 mol) of 4-chloro-5-phenoxy pyrimidine and the mixture was heated in a 250 ml. stainless steel pressure bomb at 160° for six hrs. The bomb was cooled and the contents poured into a 1000 ml. rb flask. The bomb was rinsed with 4 × 100 ml. boiling ethanol and the combined ethanol solutions were stripped to an oily mixture on the rotary evaporator. The residues were extracted with 4 × 150 ml ether and the ether solution concentrated on the steam bath until a solid began to precipitate. Cooling gave a yellow solid which was collected by vacuum filtration. The solid was taken up in hot ethyl acetate and treated with activated charcoal filtered and concentrated on the steam bath. Careful addition of hexane and cooling gave 15.3 g (66%) white crystals mp 118°-120°.

1. temperatureThe bomb was cooled
2. additionthe contents poured into a 1000 ml
3. washThe bomb was rinsed with 4 × 100 ml
4. customboiling ethanol and the combined ethanol solutions were stripped to an oily mixture on the rotary evaporator
5. extractionThe residues were extracted with 4 × 150 ml ether
6. concentrationthe ether solution concentrated on the steam bath until a solid
7. customto precipitate
8. temperatureCooling
9. customgave a yellow solid which
10. filtrationwas collected by vacuum filtration
11. additiontreated with activated charcoal
12. filtrationfiltered
13. concentrationconcentrated on the steam bath
14. additionCareful addition of hexane
15. temperaturecooling