Phosphorus oxychloride → HCID 86633413, compound

HRID 1617225Notes

Reaction equation

HRID 1617225 reaction equation
O=P(Cl)(Cl)[Cl:3].[NH2:6][C:7]1[N:12]=[C:11](O)[C:10]([CH2:14][C:15]2[CH:24]=[CH:23][C:18]([C:19]([O:21][CH3:22])=[O:20])=[CH:17][C:16]=2[O:25][CH2:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)=[C:9]([CH3:33])[N:8]=1>>[NH2:6][C:7]1[N:12]=[C:11]([Cl:3])[C:10]([CH2:14][C:15]2[CH:24]=[CH:23][C:18]([C:19]([O:21][CH3:22])=[O:20])=[CH:17][C:16]=2[O:25][CH2:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)=[C:9]([CH3:33])[N:8]=1

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 178497679HCID 178497679, compound

Product 1

HCID 86633413HCID 86633413, compound

Conditions

Temperature
80 °C

Procedure

POCl3 (25 ml) was added to the product from step (vi) (4.8 g) and stirred at 80° C. for 18 h. After cooling, the reaction was evaporated to dryness and the residue diluted with water (100 mL) and neutralized with solid NaHCO3. The mixture was heated at 50° C. for 30 min and left to cool. The subtitle compound was collected by filtration as a solid, 3.78 g.

Workup

  1. temperatureAfter cooling
  2. customthe reaction was evaporated to dryness
  3. additionthe residue diluted with water (100 mL)
  4. temperatureThe mixture was heated at 50° C. for 30 min
  5. waitleft
  6. temperatureto cool
  7. filtrationThe subtitle compound was collected by filtration as a solid, 3.78 g

Sources & evidence

ORD record
ord-bbdbe55b507b49eb82c55dc8ea0f1f4e
Source dataset
uspto-grants-2014_07
Patent number
US08765939B2

Reaction notes

Loading…