Phosphoric Acid → Phosphoric acid--azepan-2-one (1/1)

HRID 1353134Notes

Reaction equation

HRID 1353134 reaction equation
[C:1]1(=[O:8])[NH:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[P:9](=[O:13])([OH:12])([OH:11])[OH:10]>O>[P:9]([OH:13])([OH:12])([OH:11])=[O:10].[C:1]1(=[O:8])[NH:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

Participants

4

Reactant 2

HCID 1004Phosphoric AcidHCID 7768Caprolactam

Product 1

HCID 21102323Phosphoric acid--azepan-2-one (1/1)

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

To a 100 ml flask containing 11.32 g of caprolactam (0.1 mol), 30 ml water was added and stirred for dissolution. 11.53 g of 85% phosphoric acid (0.1 mol) was added dropwise into the flask over 30 min at room temperature. Then the reaction was stirred for another 12 hours. Desired product was formed after water was removed under reduced pressure and dried at 110° C. under 1–5 mmHg for 1 hour. The white, moisture- and water-stable solid of caprolactam dihydrogen phosphate was obtained with a yield of 98.6% and a melting point of 61–64° C. No glass transition temperature was observed.

Workup

  1. additionwas added
  2. stirringThen the reaction was stirred for another 12 hours

Sources & evidence

ORD record
ord-2b694a700dc7400ebb409311deecf161
Source dataset
uspto-grants-2007_05
Patent number
US07220869B2

Reaction notes

Loading…