Phosphorus oxychloride → HCID 20266877, compound

HRID 1719454Notes

Reaction equation

HRID 1719454 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

  1. customTo a three-necked flask fitted with a thermometer, distillation column and a nitrogen tube
  2. temperatureThe reaction mixture was heated
  3. temperatureto reflux under nitrogen overnight
  4. customExcess POCl3 was removed at the pump at room temperature
  5. 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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