Water → HCID 17899304, compound

HRID 275953Notes

Reaction equation

HRID 275953 reaction equation
[CH3:1][C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([F:15])=[CH:11][CH:10]=2)[N:5]=[C:4](O)[CH:3]=1.P(Cl)(Cl)([Cl:19])=O.O>ClCCl>[CH3:1][C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([F:15])=[CH:11][CH:10]=2)[N:5]=[C:4]([Cl:19])[CH:3]=1

Participants

5

Reactant 3

HCID 962WaterHCID 24813Phosphorus oxychlorideHCID 178429397HCID 178429397, compound

Product 1

HCID 17899304HCID 17899304, compoundYield 83.5%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A reaction mixture of 6-methyl-4-hydroxy-2-(4-fluorophenylamino)pyrimidine (1.74 g, 7.93 mmol) and phosphorus oxychloride was stirred for 1 hour at a room temperature and then dissolved in dichloromethane. Water was added dropwise to the reaction mixture and stirred for 30 minutes. The separated organic layer was washed with 2N NaOH solution, dried over anhydrous magnesium sulfate, and then concentrated under a reduced pressure to give 1.57 g of the titled compound. (Yield 83.5%)

Workup

  1. stirringstirred for 30 minutes
  2. washThe separated organic layer was washed with 2N NaOH solution
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under a reduced pressure

Sources & evidence

ORD record
ord-31f3a79d057b481fbbe1d25ce03cefb7
Source dataset
uspto-grants-2002_03
Patent number
US06352993B1

Reaction notes

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