Phosphorus oxychloride → HCID 20266877, compound
Reaction equation
Br.[Br:2][CH2:3][CH2:4][CH2:5][NH2:6].[O:7]=[P:8](Cl)([Cl:10])[Cl:9]>>[Br:2][CH2:3][CH2:4][CH2:5][NH:6][P:8]([Cl:10])([Cl:9])=[O:7]Participants
3
Procedure
To a three-necked flask fitted with a thermometer, distillation column and a nitrogen tube was added 3-bromopropylamine hydrobromide (12 g, 0.055 mol) and 20 mL of POCl3 (0.22 mol). The reaction mixture was heated to reflux under nitrogen overnight. Excess POCl3 was removed at the pump at room temperature (attempted distillation resulted in decomposition). The crude dichloridate, 15.4 g, was used directly in the procedure of the following Example V.
Workup
- customTo a three-necked flask fitted with a thermometer, distillation column and a nitrogen tube
- temperatureThe reaction mixture was heated
- temperatureto reflux under nitrogen overnight
- customExcess POCl3 was removed at the pump at room temperature
- distillation(attempted distillation resulted in decomposition)
Sources & evidence
- ORD record
- ord-af1fa63e0dca49148002ca4ea144e27a
- Source dataset
- uspto-grants-1985_09
- Patent number
- US04540428
Reaction notes
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