反应详情

A mixture of 2,6-dimethyl-5-iodo-4-hydroxypyrimidine (24.5 g, 0.098 mol), phosphorus oxychloride (30.0 g, 0.196 mol) and toluene (200 mL) was heated under reflux for 1 h. The mixture was concentrated and ice water (100 mL) was added. The pH was adjusted to 5 with 2.5N NaOH and the mixture was extracted with CH2Cl2. The combined extracts were washed with brine, dried MgSO4), and concentrated to give 24.6 g of a brown solid. The crude product was combined with 26.0 g of similarly prepared material and filtered through a short column of silica gel eluted with CH2Cl2 to give 33.8 g (62%) of product as a yellow solid. An analytical sample was recrystallized from hexane/CH2Cl2, mp 62°-64° C.

1. temperaturewas heated
2. temperatureunder reflux for 1 h
3. concentrationThe mixture was concentrated
4. additionice water (100 mL) was added
5. extractionthe mixture was extracted with CH2Cl2
6. washThe combined extracts were washed with brine, dried MgSO4), and
7. concentrationconcentrated