Sodium Methoxide → HCID 15008938, compound
Reaction equation
[CH3:1][O-:2].[Na+].[CH3:4][NH:5][C:6]1[N:11]=[C:10](C(Cl)(Cl)Cl)[N:9]=[C:8]([C:16]([F:19])([F:18])[F:17])[N:7]=1>CO.O.Cl>[CH3:1][O:2][C:10]1[N:11]=[C:6]([NH:5][CH3:4])[N:7]=[C:8]([C:16]([F:19])([F:18])[F:17])[N:9]=1Participants
Procedure
21.8 g of a 30% strength solution of sodium methanolate in methanol (0.12 mol of sodium methanolate) were added dropwise to a solution of 119.4 g (0.40 mol) of 2-methylamino-4-trichloromethyl-6-trifluoromethyl-1,3,5-triazine in 400 ml of methanol. The resulting yellow mixture was then refluxed for 1 hour during which it gradually became cloudy. After addition of a further 7.2 g of the 30% strength solution of sodium methanolate in methanol (0.04 mol of sodium methanolate), the mixture was refluxed for a further 30 minutes and, after cooling to 20° to 25° C., diluted with 150 ml of water and neutralized with 1 normal aqueous hydrochloric acid. The solvent was then removed at 40° C. under reduced pressure, after which the resulting solid was separated off and dried at 40° C. under reduced pressure for 15 hours.
Workup
- temperatureThe resulting yellow mixture was then refluxed for 1 hour during which it gradually became cloudy
- temperaturethe mixture was refluxed for a further 30 minutes
- temperatureafter cooling to 20° to 25° C.
- customThe solvent was then removed at 40° C. under reduced pressure
- customafter which the resulting solid was separated off
- customdried at 40° C. under reduced pressure for 15 hours
Sources & evidence
- ORD record
- ord-412da58d239e4001a5a6c6a8595d92ff
- Source dataset
- uspto-grants-1992_07
- Patent number
- US05130428
Reaction notes
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