Ethanol → HCID 67783752, compound

HRID 2082263Notes

Reaction equation

HRID 2082263 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% strength sodium hydride were added a little at a time to 150 ml of ethanol at from 20 to 35° C. and stirring was carried out until dissolution occurred, which took 15 minutes. 10.0 g (0.047 mol) of 2-amino-4-chlorodifluoromethoxy-6-fluoro-1,3,5-triazine were then added at 0° C., while stirring, and stirring was continued for 1 hour at 0° C. and overnight at 22° C. The solution was evaporated down under reduced pressure, after which the residue was taken up in methylene chloride and the solution was extracted with water and dried. Evaporation gave 10.6 g (94.6% of theory) of the title compound of melting point 63°-65° C.

Workup

  1. dissolutionwas carried out until dissolution
  2. stirringwhile stirring
  3. stirringstirring
  4. waitwas continued for 1 hour at 0° C. and overnight at 22° C
  5. customThe solution was evaporated down under reduced pressure
  6. extractionthe solution was extracted with water
  7. customdried
  8. customEvaporation

Sources & evidence

ORD record
ord-7857a065735b437bae1074af9a138498
Source dataset
uspto-grants-1993_02
Patent number
US05188657

Reaction notes

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