Phosphorus oxychloride → HCID 57799710, compound

HRID 2100749Notes

Reaction equation

HRID 2100749 reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[C:11]([O:13][CH3:14])[CH:12]=1)[C:9](O)=[N:8][C:7]([NH:16][C:17]1[CH:21]=[C:20]([CH3:22])[NH:19][N:18]=1)=[CH:6]2.O=P(Cl)(Cl)[Cl:25]>>[Cl:25][C:9]1[C:10]2[C:5](=[CH:4][C:3]([O:2][CH3:1])=[CH:12][C:11]=2[O:13][CH3:14])[CH:6]=[C:7]([NH:16][C:17]2[CH:21]=[C:20]([CH3:22])[NH:19][N:18]=2)[N:8]=1

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 178493402HCID 178493402, compound

Product 1

HCID 57799710HCID 57799710, compoundYield 47.28%

Conditions

Temperature
140 °C

Procedure

A mixture of 6,8-Dimethoxy-3-(5-methyl-1H-pyrazol-3-ylamino)-isoquinolin-1-ol (0.4 g, 1.33 mmol) in POCl3 (4 ml), were sealed in microwave process vials (5 ml). The mixture was heated at 140° C. for 75 minutes under microwave irradiation. The mixture was concentrated, and the residue was treated with 1 ml MeOH. The solid was collected and dried to give desired product (0.2 g, 47.28%). LC-MS: m/e 319 (MH+).

Workup

  1. customwere sealed in microwave process vials (5 ml)
  2. concentrationThe mixture was concentrated
  3. additionthe residue was treated with 1 ml MeOH
  4. customThe solid was collected
  5. customdried

Sources & evidence

ORD record
ord-f0eb0b0ec5114e9988a4b638e4deaa1d
Source dataset
uspto-grants-2009_08
Patent number
US07572809B2

Reaction notes

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