Phosphorus oxychloride → HCID 74220733, compound

HRID 2205835Notes

Reaction equation

HRID 2205835 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-576a92bcf3b24c578e2f3302349fa0b2
Source dataset
uspto-grants-2016_06
Patent number
US09371332B2

Reaction notes

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