Ammonia → HCID 45078476, compound
Reaction equation
[CH3:1][O:2][C:3]1[C:11]2[NH:10][C:9](=O)[N:8]([CH3:13])[C:7]=2[CH:6]=[CH:5][CH:4]=1.N.P(Cl)(Cl)([Cl:17])=O>>[Cl:17][C:9]1[N:8]([CH3:13])[C:7]2[CH:6]=[CH:5][CH:4]=[C:3]([O:2][CH3:1])[C:11]=2[N:10]=1Participants
4
Procedure
3.7 g 4-methoxy-1-methyl-1,3-dihydrobenzimidazol-2-one are suspended in 15 ml phosphorus oxychloride. The reaction mixture is stirred for 3 hours at reflux temperature, slowly combined with ice water and made alkaline with conc. ammonia. The precipitated product is suction filtered. 3.6 g product are obtained as a solid. M.p=118-119° C.
Workup
- temperatureat reflux temperature
- filtrationfiltered
Sources & evidence
- ORD record
- ord-293bb8cfc3af4680add50ed0e8a58f31
- Source dataset
- uspto-grants-2014_11
- Patent number
- US08877758B2
Reaction notes
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