Phosphorus oxychloride → HCID 74220733, compound

HRID 588632Notes

Reaction equation

HRID 588632 reaction equation
[I:1][C:2]1[N:7]=[N:6][C:5]2[N:8]([CH3:17])[N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[C:4]=2[C:3]=1O.P(Cl)(Cl)([Cl:21])=O>>[Cl:21][C:3]1[C:2]([I:1])=[N:7][N:6]=[C:5]2[N:8]([CH3:17])[N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[C:4]=12

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 178481731HCID 178481731, compound

Product 1

HCID 74220733HCID 74220733, compound

Procedure

5-Iodo-1-methyl-3-phenyl-pyrazolo[3,4-c]pyridazin-4-ol (160 mg, 0.45 mmol) in phosphorous oxychloride (0.6 mL) was heated to 120° C. for 10 min. The reaction mixture was cooled to room temperature and the suspension was filtered. The collected solid was dissolved in CH2Cl2 and washed with water. The organic phase was dried (phase separator cartridge) and concentrated in vacuo, to yield Compound IIIa (130 mg).

Workup

  1. filtrationthe suspension was filtered
  2. dissolutionThe collected solid was dissolved in CH2Cl2
  3. washwashed with water
  4. customThe organic phase was dried (phase separator cartridge)
  5. concentrationconcentrated in vacuo
  6. customto yield Compound IIIa (130 mg)

Sources & evidence

ORD record
ord-8395db10ed0342a4ab17ce1379ff4a7b
Source dataset
uspto-grants-2016_01
Patent number
US09227976B2

Reaction notes

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