Water → HCID 60726868, compound

HRID 1846424Notes

Reaction equation

HRID 1846424 reaction equation
[H-].[Na+].[CH3:3][C:4]1[CH:5]=[C:6]([OH:11])[CH:7]=[CH:8][C:9]=1[CH3:10].[Cl:12][C:13]1[CH:18]=[C:17](Cl)[N:16]=[CH:15][N:14]=1.O>CN(C=O)C.CCOC(C)=O>[Cl:12][C:13]1[CH:18]=[C:17]([O:11][C:6]2[CH:7]=[CH:8][C:9]([CH3:10])=[C:4]([CH3:3])[CH:5]=2)[N:16]=[CH:15][N:14]=1

Participants

7

Reactant 4

HCID 962WaterHCID 72493,4-DimethylphenolHCID 24758Sodium hydrideHCID 709434,6-Dichloropyrimidine

Product 1

HCID 60726868HCID 60726868, compound

Reagents, catalysts & solvents 2

HCID 6228DimethylformamideSolventHCID 8857Ethyl AcetateSolvent

Procedure

218 mg (5.00 mmol) sodium hydride (55%, suspension in mineral oil) were added to 617 mg (5.00 mmol) 3,4-dimethylphenol in 10 ml DMF and the mixture was stirred for 10 min at RT. Then 768 mg (5.00 mmol) 4,6-dichloropyrimidine were added and the mixture was stirred for 48 h at RT. Water and EtOAc were added to the reaction mixture, the organic phase was separated off, dried on sodium sulphate, filtered and evaporated down. The residue was dried i. vac.

Workup

  1. stirringthe mixture was stirred for 48 h at RT
  2. customthe organic phase was separated off
  3. customdried on sodium sulphate
  4. filtrationfiltered
  5. customevaporated down
  6. customThe residue was dried i

Sources & evidence

ORD record
ord-dae408575d6a407bafdba33d852afa0f
Source dataset
uspto-grants-2015_02
Patent number
US08952014B2

Reaction notes

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