Phosphorus oxychloride → HCID 18381670, compound

HRID 2268876Notes

Reaction equation

HRID 2268876 reaction equation
[CH3:1][O:2][C:3]1[C:4]([C:14]#[C:15][CH2:16][CH2:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=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:27]>C(Cl)Cl>[Cl:27][C:9]1[C:10]2[C:5](=[C:4]([C:14]#[C:15][CH2:16][CH2:17][CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=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 18381656HCID 18381656, compound

Product 1

HCID 18381670HCID 18381670, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Conditions

Temperature
80 °C

Procedure

A suspension of 6-methoxy-5-(5-phenyl-pent-1-ynyl)-2H-phthalazin-1-one (1.26 g, 3.96 mmoles), prepared as described in example 64, and POCl3 (30 ml) was heated at 80° C. under stirring up to dissolution. After 30 minutes the solution was brought to dryness, the residue dissolved in CH2Cl2, washed to alkalinity with a diluted solution of K2CO3, then with water, anhydrified over Na2SO4 and brought to dryness to give 1.33 g of the title compound (quantitative yield). The compound was used as such in the subsequent step.

Workup

  1. customprepared
  2. washwashed

Sources & evidence

ORD record
ord-fa001b5d7ad24e03b3f30021c927cd81
Source dataset
uspto-grants-2001_12
Patent number
US06329370B1

Reaction notes

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