Dimethylformamide → HCID 13672005, compound

HRID 1905846Notes

Reaction equation

HRID 1905846 reaction equation
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[N:5]=[C:4]([SH:9])[N:3]=1.C(=O)([O-])[O-].[K+].[K+].CN(C)C=O.Cl[CH:22]([F:24])[F:23]>O>[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[N:5]=[C:4]([S:9][CH:22]([F:24])[F:23])[N:3]=1

Participants

6

Reactant 4

HCID 6228DimethylformamideHCID 6372ChlorodifluoromethaneHCID 11430Potassium CarbonateHCID 178508836HCID 178508836, compound

Product 1

HCID 13672005HCID 13672005, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To a mixture of 2.8 g of 2,4-diamino-6-mercapto-1,3,5-triazine, 5.5 g of potassium carbonate, and 20 ml of N,N-dimethylformamide is added and chlorodifluoromethane gas is aspirated at a temperature of 55°~65° C. for 2 hours in a 100 ml three-necked flask. After cooling, the mixture is mixed with water and extracted with ethyl acetate. The extract is evaported, and the resulting residue is purified by silica-gel chromatography to produce 0.8 g of 2,4-diamino-6-difluoromethylthio-1,3,5-triazine.

Workup

  1. additionis added
  2. temperatureAfter cooling
  3. extractionextracted with ethyl acetate
  4. customthe resulting residue is purified by silica-gel chromatography

Sources & evidence

ORD record
ord-78de3ac06b99436c9d0dca0dc5bf721a
Source dataset
uspto-grants-1987_03
Patent number
US04648898

Reaction notes

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