Phosphorus oxychloride → 4-Chloro-5-iodo-6-methylpyrimidine
Reaction equation
O[C:2]1[C:7]([I:8])=[C:6]([CH3:9])[N:5]=[CH:4][N:3]=1.O=P(Cl)(Cl)[Cl:12]>>[Cl:12][C:2]1[C:7]([I:8])=[C:6]([CH3:9])[N:5]=[CH:4][N:3]=1Participants
3
Conditions
- Temperature
- 90 °C
Procedure
A suspension of 90 g (0.38 mol) 4-hydroxy-5-iodo-6-methyl pyrimidine in 600 mL POCl3 is heated for 1 h at 90° C. The reaction mixture is concentrated under reduced pressure and the residue is poured into crushed ice. The precipitated solid is collected by filtration and washed with water. After drying, the desired product is obtained as a solid (90 g; 93%).
Workup
- concentrationThe reaction mixture is concentrated under reduced pressure
- additionthe residue is poured
- custominto crushed ice
- filtrationThe precipitated solid is collected by filtration
- washwashed with water
- customAfter drying
Sources & evidence
- ORD record
- ord-c26e4091181c4c0782e2c342503a9e4e
- Source dataset
- uspto-grants-2013_12
- Patent number
- US08618111B2
Reaction notes
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