Sodium Hydroxide → HCID 178493216, compound
Reaction equation
Cl[O-].[Na+].[OH-].[Na+].[CH3:6][O:7][C:8]1[CH:13]=[CH:12][N:11]=[C:10]([CH2:14][S:15][C:16]2[NH:20][C:19]3[CH:21]=[CH:22][C:23]([O:25][C:26]([F:31])([F:30])[CH:27]([F:29])[F:28])=[CH:24][C:18]=3[N:17]=2)[CH:9]=1.S([O-])([O-])(=[O:34])=S.[Na+].[Na+].S([O-])([O-])(=O)=O.[NH4+].[NH4+]>C(OCC)(=O)C>[CH3:6][O:7][C:8]1[CH:13]=[CH:12][N:11]=[C:10]([CH2:14][S:15]([C:16]2[NH:20][C:19]3[CH:21]=[CH:22][C:23]([O:25][C:26]([F:31])([F:30])[CH:27]([F:29])[F:28])=[CH:24][C:18]=3[N:17]=2)=[O:34])[CH:9]=1Participants
Procedure
A mixture of 8.5 ml of commercially available sodium hypochlorite solution (about 15% of active chlorine) and 6 ml of 10% strength sodium hydroxide solution is added dropwise to a solution of 1.5 g 2-[(4-methoxy-2-pyridyl)methylthio]-5-(1,1,2,2-tetrafluoroethoxy)-1H-benzimidazole in 30 ml of ethyl acetate at 0° C. in the course of 20 min., stirring is continued at this temperature for 20 min. and 0.6 ml of 10% strength sodium thiosulfate solution is then added. 1.5 g of ammonium sulfate are added and the organic phase is separated off, washed with saturated sodium chloride solution, dried with magnesium sulfate and concentrated to a small volume. 1.3 g (85%) of the title compound of melting point 131°-132° C. (decomposition) are obtained by precipitation with diisopropyl ether.
Workup
- customthe organic phase is separated off
- washwashed with saturated sodium chloride solution
- dry with materialdried with magnesium sulfate
- concentrationconcentrated to a small volume
Sources & evidence
- ORD record
- ord-b7f778150f854f568c2c70dd1fdb0e85
- Source dataset
- uspto-grants-1985_11
- Patent number
- US04555518
Reaction notes
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