Phosphorus oxychloride → HCID 19096775, compound

HRID 486875Notes

Reaction equation

[Cl:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([NH:10][C:11](=O)[CH2:12][Cl:13])=[C:4]([F:15])[CH:3]=1.P(Cl)(Cl)(Cl)(Cl)[Cl:17].P(Cl)(Cl)(Cl)=O>>[Cl:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([N:10]=[C:11]([Cl:17])[CH2:12][Cl:13])=[C:4]([F:15])[CH:3]=1

Participants

Reactant 3

HCID 24813Phosphorus oxychloride

HCID 24819Phosphorus pentachloride

HCID 19096771HCID 19096771, compound

Product 1

HCID 19096775HCID 19096775, compoundYield 78.3%

Procedure

First, 2.00 g of N-(4-chloro-2-fluoro-5-methoxyphenyl)-2-chloroacetamide was mixed with 1.66 g of phosphorus pentachloride, and the stirring was continued for 1.0 hr at 60° C. After letting the mixture stand to cool the same, the produced phosphorus oxychloride was distilled out under reduced pressure. Then, the residue was refined by vacuum distillation to obtain 1.68 g of N-(4-chloro-2-fluoro-5-methoxyphenyl)-2-chloroacetimidoylchloride. The boiling point was 121° C./0.5 mm Hg.

Workup

distillationwas distilled out under reduced pressure
distillationThen, the residue was refined by vacuum distillation

Sources & evidence

ORD record: ord-b5b4d591cd124bf4a3a1d21fab8e59cc
Source dataset: uspto-grants-1994_03
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US05292922

Reaction notes

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