Carbon Tetrachloride → HCID 14718738, compound

HRID 1085705Notes

Reaction equation

HRID 1085705 reaction equation
[CH3:1][C:2]([C:5]1[N:10]=[CH:9][C:8]([C:11](=O)[C:12]([F:15])([F:14])[F:13])=[CH:7][N:6]=1)([CH3:4])[CH3:3].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[C:36](Cl)(Cl)([Cl:38])[Cl:37]>>[Cl:37][C:36]([Cl:38])=[C:11]([C:8]1[CH:7]=[N:6][C:5]([C:2]([CH3:4])([CH3:3])[CH3:1])=[N:10][CH:9]=1)[C:12]([F:15])([F:14])[F:13]

Participants

4

Reactant 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 14718737HCID 14718737, compound

Product 1

HCID 14718738HCID 14718738, compound

Procedure

2-(1,1-dimethylethyl-5-trifluoroacetylpyrimidine (0.9 g) was dissolved in dry carbon tetrachloride (15 cm3) containing triphenylphosphine (2.5 g). The reaction mixture was stirred under a nitrogen atmosphere and heated at the reflux temperature for 30 hours to give a deep red-brown solution. The reaction mixture was fractioned by filtering the cooled solution through a short column of silica gel and eluting with a mixture of hexane/dichloromethane (3:1 by volume). On evaporation of the solvents the product was obtained as a colourless solid (0.9 g)

Workup

  1. temperatureheated at the reflux temperature for 30 hours
  2. customto give a deep red-brown solution
  3. filtrationby filtering the cooled solution through a short column of silica gel
  4. washeluting with a mixture of hexane/dichloromethane (3:1 by volume)
  5. customOn evaporation of the solvents the product

Sources & evidence

ORD record
ord-6b725fd37cae46cd9d0b1304e5120784
Source dataset
uspto-grants-1991_04
Patent number
US05010200

Reaction notes

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