Phosphorus oxychloride → HCID 20241991, compound

HRID 1380059Notes

Reaction equation

HRID 1380059 reaction equation
[I:1][C:2]1[CH:3]=[C:4]([C:8]2[NH:9][CH:10]=[CH:11][C:12](=O)[N:13]=2)[CH:5]=[CH:6][CH:7]=1.P(Cl)(Cl)([Cl:17])=O>>[Cl:17][C:12]1[CH:11]=[CH:10][N:9]=[C:8]([C:4]2[CH:5]=[CH:6][CH:7]=[C:2]([I:1])[CH:3]=2)[N:13]=1

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 178516533HCID 178516533, compound

Product 1

HCID 20241991HCID 20241991, compound

Procedure

A 32.9 g portion of 2-(3-iodophenyl)-4(1H)-pyrimidinone was stirred and refluxed in 123 ml. of phosphorus oxychloride for 2 hours, then cooled overnight and the solvent evaporated at 55° C. The residue was suspended in 400 ml of chloroform, then evaporated. This residue was taken up in 300 ml of chloroform, filtered and washed twice with 75 ml of chloroform. The combined filtrate and washes were evaporated giving 4-chloro-2-(3-iodophenyl)pyrimidine.

Workup

  1. temperaturerefluxed in 123 ml
  2. temperaturecooled overnight
  3. customthe solvent evaporated at 55° C
  4. customevaporated
  5. filtrationfiltered
  6. washwashed twice with 75 ml of chloroform
  7. customThe combined filtrate and washes were evaporated

Sources & evidence

ORD record
ord-8921604f5f1346fd8f23869052f9b357
Source dataset
uspto-grants-1986_04
Patent number
US04579848

Reaction notes

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