Ethanol → HCID 67783752, compound

HRID 1198285Notes

Reaction equation

HRID 1198285 reaction equation
[H-].[Na+].[NH2:3][CH:4]1[N:9]=[C:8]([Cl:10])[N:7]=[C:6](F)[N:5]1[O:12][CH:13]([F:15])[F:14].[CH2:16]([OH:18])[CH3:17]>>[NH2:3][CH:4]1[N:9]=[C:8]([Cl:10])[N:7]=[C:6]([O:18][CH2:16][CH3:17])[N:5]1[O:12][CH:13]([F:15])[F:14]

Participants

4

Reactant 3

HCID 702EthanolHCID 24758Sodium hydrideHCID 67783290HCID 67783290, compound

Product 1

HCID 67783752HCID 67783752, compound

Procedure

1.2 g (0.047 mol) of 97% sodium hydride were added a little at a time to 150 ml of ethanol at 20°-35° C. and dissolved by stirring for 15 minutes. Then while stirring at 0° C., 10.0 g (0.047 mol) of 2-amino-4-chlorodifluoromethoxy-6-fluoro-1,3,5-triazine were added, and the mixture was stirred at 0° C. for 1 hour and at 22° C. overnight. The residue from concentration under reduced pressure was taken up in methylene chloride, extracted with water and dried. Concentration yielded 10.6 g (94.6% of theory) of the title compound of melting point 63°-65° C.

Workup

  1. dissolutiondissolved
  2. stirringThen while stirring at 0° C.
  3. stirringthe mixture was stirred at 0° C. for 1 hour and at 22° C. overnight
  4. concentrationThe residue from concentration under reduced pressure
  5. extractionextracted with water
  6. customdried
  7. concentrationConcentration

Sources & evidence

ORD record
ord-27a00fbd79be47439b7b84b685810a9a
Source dataset
uspto-grants-1994_01
Patent number
US05280118

Reaction notes

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