反应详情

To 500 ml. of phosphorus oxychloride was added 85.5 g. (0.455 mol) of 4-hydroxy-5-phenoxy pyrimidine and the suspension heated at 70° in an oil bath. After 1 hr the reaction mixture became homogeneous and after 1.5 hr total reduction time the bulk of the phosphorus oxychloride was removed by distillation at reduced pressure. The residue was slowly added to well stirred iced water and the residual acid was cautiously neutralized with ammonium hydroxide solution to pH 8 and was extracted with 3 × 700 ml. of chloroform. The chloroform extracts were dried over anhydrous sodium sulfate filtered and concentrated in vacuo to 85.7 g. (90%) of a black oil. A colorless oil could be obtained by evaporative distillation of this material at 130° (0.1 mm).

1. customtotal reduction time the bulk of the phosphorus oxychloride was removed by distillation at reduced pressure
2. additionThe residue was slowly added to well stirred iced water
3. extractionwas extracted with 3 × 700 ml
4. dry with materialThe chloroform extracts were dried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo to 85.7 g
7. customA colorless oil could be obtained by evaporative distillation of this material at 130° (0.1 mm)