Triethylsilane → HCID 15346138, compound

HRID 1106456Notes

Reaction equation

HRID 1106456 reaction equation
C([SiH](CC)CC)C.[Cl:8][C:9]1[CH:14]=[CH:13][C:12]([N:15]2[C:20](=[O:21])[CH:19]=[C:18]([C:22]([F:25])([F:24])[F:23])[N:17]([CH3:26])[C:16]2=[O:27])=[CH:11][C:10]=1[CH:28]=[N:29][O:30][CH3:31]>ClCCl.FC(F)(F)C(O)=O>[Cl:8][C:9]1[CH:14]=[CH:13][C:12]([N:15]2[C:20](=[O:21])[CH:19]=[C:18]([C:22]([F:23])([F:24])[F:25])[N:17]([CH3:26])[C:16]2=[O:27])=[CH:11][C:10]=1[CH2:28][NH:29][O:30][CH3:31]

Participants

5

Reactant 2

HCID 12052TriethylsilaneHCID 54570928HCID 54570928, compound

Product 1

HCID 15346138HCID 15346138, compound

Reagents, catalysts & solvents 2

HCID 6344DichloromethaneSolventHCID 6422Trifluoroacetic acidSolvent

Procedure

Triethylsilane (1.9 ml) was added dropwise to a solution of 3-(4-chloro-3-methoxyiminomethylphenyl)-1-methyl-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione (3.6 g) in a mixture of 30 ml of dichloromethane and 50 ml of trifluoroacetic acid. After the mixture had been stirred for 20 hours at room temperature, the solvent was distilled off. The residue was taken up in 200 ml of dichloromethane, whereupon the organic phase was washed four times using 50 ml of water in each case, dried over sodium sulfate and finally concentrated. Crystallization using diisopropyl ether and petroleum ether gave the title compound (m.p. 83-85° C.).

Workup

  1. distillationthe solvent was distilled off
  2. washwas washed four times
  3. dry with materialdried over sodium sulfate
  4. concentrationfinally concentrated
  5. customCrystallization

Sources & evidence

ORD record
ord-90575abbbd0b4ae3b8635600042a9efc
Source dataset
uspto-grants-2000_05
Patent number
US06057269

Reaction notes

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