Phosphorus oxychloride → 4,5-Dichloro-6-ethylpyrimidine

Temperature

100 °C

A mixture of 3.19 g (0.020 mol) of 5-chloro-4-ethyl-6-hydroxypyrimidine, 15.33 g (0.10 mol) of phosphoryl chloride and 45 g of toluene was heated to 100° C. and stirred at this temperature for 80 minutes. The excess phosphoryl chloride and the toluene were distilled off and the residue was mixed with 30 ml of dichloromethane and 20 ml of water. The mixture was refluxed after 30 minutes, extracted with 3×30 ml of dichloromethane and dried on sodium sulfate. The dichloromethane solution was evaporated and the residue was distilled at 125° C./12 torr in the bulb tube apparatus. The following data concerns the product of this example:

1. distillationThe excess phosphoryl chloride and the toluene were distilled off
2. additionthe residue was mixed with 30 ml of dichloromethane and 20 ml of water
3. temperatureThe mixture was refluxed after 30 minutes
4. extractionextracted with 3×30 ml of dichloromethane
5. customdried on sodium sulfate
6. customThe dichloromethane solution was evaporated
7. distillationthe residue was distilled at 125° C./12 torr in the bulb tube apparatus

ORD record

ord-de7e17129441450a8ebb196297830745

Source dataset

uspto-grants-1990_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04977264