Phosphorus oxychloride → HCID 68867784, compound

HRID 1986593Notes

Reaction equation

HRID 1986593 reaction equation
[CH3:1][O:2][N:3]1[CH:20]=[C:6]2[CH:7]=[N:8][C:9]3[C:14](=O)[C:13]([CH3:16])=[CH:12][N:11]([CH2:17][CH2:18][CH3:19])[C:10]=3[N:5]2[CH2:4]1.O=P(Cl)(Cl)[Cl:23]>>[Cl:23][C:14]1[C:9]2[N:8]=[CH:7][C:6]3[N:5]([CH2:4][N:3]([O:2][CH3:1])[CH:20]=3)[C:10]=2[N:11]([CH2:17][CH2:18][CH3:19])[CH2:12][C:13]=1[CH3:16]

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 68870278HCID 68870278, compound

Product 1

HCID 68867784HCID 68867784, compound

Procedure

16 g of 8-methoxy-3-methyl-1-propyl-imidazo[1,5-a]pyrido[3,2-e]pyrazine-4-one and 120 ml POCl3 are mixed and heated up to reflux for 8 hours. After cooling to room temperature the reaction mixture is treated with 1200 ml crushed ice/water and stirred for 1 hour. The product is extracted with 2×300 ml dichloromethane. The collected organic layer is washed with 2×300 ml water and dried with Na2SO4. The solvent is removed under reduced pressure.

Workup

  1. temperatureheated up
  2. temperatureto reflux for 8 hours
  3. additionis treated with 1200 ml
  4. extractionThe product is extracted with 2×300 ml dichloromethane
  5. washThe collected organic layer is washed with 2×300 ml water
  6. dry with materialdried with Na2SO4
  7. customThe solvent is removed under reduced pressure

Sources & evidence

ORD record
ord-471339212c1c4f1dbb86ed45a1bb1c20
Source dataset
uspto-grants-2009_06
Patent number
US07550465B2

Reaction notes

Loading…