Phosphorus oxychloride → HCID 11232044, compound
Reaction equation
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:12]=[CH:11][C:10]([N+:13]([O-:15])=[O:14])=[CH:9][C:8]=2[S:16]([O-:19])(=O)=[O:17])[CH2:3][CH2:2]1.[Na+].P(Cl)(Cl)([Cl:23])=O>C(#N)C>[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:12]=[CH:11][C:10]([N+:13]([O-:15])=[O:14])=[CH:9][C:8]=2[S:16]([Cl:23])(=[O:19])=[O:17])[CH2:3][CH2:2]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
31 g (0.1 mol) of sodium 2-morpholino-5-nitrobenzenesulfonate obtained in Step (a) above and 60 ml (0.67 mol) of phosphorus oxychloride were added to 300 ml of acetonitrile and the mixture was refluxed by heating for 2 hours. After cooling, the reaction mixture was added to 600 ml of ice water. The crystals thus-precipitated were collected by filtration. Yield: 18.5 g (60%).
Workup
- temperaturethe mixture was refluxed
- temperatureby heating for 2 hours
- temperatureAfter cooling
- customThe crystals thus-precipitated
- filtrationwere collected by filtration
Sources & evidence
- ORD record
- ord-cf063727e7894c9e9c726396a152be46
- Source dataset
- uspto-grants-1984_09
- Patent number
- US04473632
Reaction notes
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