Phosphorus oxychloride → HCID 57799845, compound

HRID 2101123Notes

Reaction equation

HRID 2101123 reaction equation
[CH3:1][O:2][C:3]1[C:4]([CH3:21])=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9](=O)[NH:8][C:7]([NH:14][C:15]1[CH:19]=[C:18]([CH3:20])[NH:17][N:16]=1)=[CH:6]2.O=P(Cl)(Cl)[Cl:24]>>[Cl:24][C:9]1[C:10]2[C:5](=[C:4]([CH3:21])[C:3]([O:2][CH3:1])=[CH:12][CH:11]=2)[CH:6]=[C:7]([NH:14][C:15]2[CH:19]=[C:18]([CH3:20])[NH:17][N:16]=2)[N:8]=1

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 57799646HCID 57799646, compound

Product 1

HCID 57799845HCID 57799845, compound

Conditions

Temperature
150 °C

Procedure

A 10˜20 mL process vial was charged with 500 mg 6-Methoxy-5-methyl-3-(5-methyl-1H-pyrazol-3-ylamino)-2H-isoquinolin-1-one in 15 mL POCl3. The vial was heated at 150° C. for 30 min under microwave irradiation. After cooling, POCl3 was removed under reduced pressure. MeOH was carefully added to the residue during which the precipitate was formed. The solid was collected as crude product for the next reaction.

Workup

  1. temperatureAfter cooling
  2. customPOCl3 was removed under reduced pressure
  3. additionMeOH was carefully added to the residue during which the precipitate
  4. customwas formed
  5. customThe solid was collected as crude product for the next reaction

Sources & evidence

ORD record
ord-582cc45158e744cdacc5315f3b61a675
Source dataset
uspto-grants-2009_08
Patent number
US07572809B2

Reaction notes

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