Phosphorus oxychloride → HCID 54335011, compound

HRID 2297442Notes

Reaction equation

HRID 2297442 reaction equation
[CH3:1][O:2][C:3]1[C:4]([C:14]#[C:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9](=O)[NH:8][N:7]=[CH:6]2.O=P(Cl)(Cl)[Cl:24]>C(Cl)Cl>[Cl:24][C:9]1[C:10]2[C:5](=[C:4]([C:14]#[C:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[C:3]([O:2][CH3:1])=[CH:12][CH:11]=2)[CH:6]=[N:7][N:8]=1

Participants

4

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 53839973HCID 53839973, compound

Product 1

HCID 54335011HCID 54335011, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Conditions

Temperature
80 °C

Procedure

A suspension of 6-methoxy-5-phenylethynyl-2H-phthalazin-1-one (0.67 g, 2.42 mmoles), prepared as described in example 60, in POCl3 (20 ml) was heated at 80° C. under stirring up to dissolution. After 30 minutes the solution was brought to dryness and the residue taken up in CH2Cl2 (100 ml), washed to alkalinity with a solution of K2CO3, then with water, then anhydrified over Na2SO4 and evaporated to give 715 mg of the title compound (quantitative yield). The compound was used as such in the subsequent step.

Workup

  1. customprepared
  2. washwashed
  3. customevaporated

Sources & evidence

ORD record
ord-2e58affd6dfb4a84b21d3c7897a936b2
Source dataset
uspto-grants-2002_12
Patent number
US06492360B1

Reaction notes

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