Ethanol → HCID 67783752, compound

HRID 1647669Notes

Reaction equation

HRID 1647669 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 a solution was obtained, 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 one hour at 0° C. and overnight at 22° C. The mixture 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. Evaporating down gave 10.6 g (94.6% of theory) of the title compound of melting point 63°-65° C.

Workup

  1. customwas obtained
  2. stirringwhile stirring
  3. stirringstirring
  4. waitwas continued for one hour at 0° C. and overnight at 22° C
  5. customThe mixture was evaporated down under reduced pressure
  6. extractionthe solution was extracted with water
  7. customdried
  8. customEvaporating

Sources & evidence

ORD record
ord-67b66a4777a6451f9b3c0f28d29fec78
Source dataset
uspto-grants-1995_07
Patent number
US05434124

Reaction notes

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