Water → HCID 14276128, compound

HRID 1165199Notes

Reaction equation

HRID 1165199 reaction equation
[H-].[Na+].[F:3][C:4]([F:14])([F:13])[C:5]1[CH:12]=[CH:11][C:8]([CH2:9][OH:10])=[CH:7][CH:6]=1.[Br:15][C:16]1[C:17](=[O:24])[N:18]([CH3:23])[CH:19]=[N:20][C:21]=1Cl.O>O1CCOCC1>[Br:15][C:16]1[C:17](=[O:24])[N:18]([CH3:23])[CH:19]=[N:20][C:21]=1[O:10][CH2:9][C:8]1[CH:11]=[CH:12][C:5]([C:4]([F:13])([F:14])[F:3])=[CH:6][CH:7]=1

Participants

6

Reactant 4

HCID 962WaterHCID 24758Sodium hydrideHCID 676844-(Trifluoromethyl)benzenemethanolHCID 15058925117113-95-8

Product 1

HCID 14276128HCID 14276128, compoundYield 88.2%

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

Sodium hydride (55% in mineral oil) (0.22 g) was suspended in 10 ml of dioxane, and then 0.88 g of 4-trifluoromethylbenzyl alcohol was added thereto. The resulting mixture was stirred for one hour at room temperature, then incorporated with 1.12 g of 5-bromo-6-chloro-3-methyl-4(3H)-pyrimidinone and stirred for 15 hours. The resulting solution was poured into water, and the resulting crystals were filtered off and then recrystallized from a benzene-hexane mixture to give 1.60 g of the intended product.

Workup

  1. stirringstirred for 15 hours
  2. filtrationthe resulting crystals were filtered off
  3. customrecrystallized from a benzene-hexane mixture

Sources & evidence

ORD record
ord-54e342ff338545b195c92f308ce9f6f5
Source dataset
uspto-grants-1990_03
Patent number
US04908379

Reaction notes

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