Phosphorus oxychloride → HCID 54085186, compound

HRID 1578955Notes

Reaction equation

HRID 1578955 reaction equation
[CH2:1]([O:3][C:4](=[O:20])[CH2:5][S:6][C:7]1[N:12]=[C:11](O)[CH:10]=[C:9]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:8]=1)[CH3:2].P(Cl)(Cl)([Cl:23])=O>>[CH2:1]([O:3][C:4](=[O:20])[CH2:5][S:6][C:7]1[N:12]=[C:11]([Cl:23])[CH:10]=[C:9]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:8]=1)[CH3:2]

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 178473169HCID 178473169, compound

Product 1

HCID 54085186HCID 54085186, compound

Procedure

A solution of 18.0 g of (4-hydroxy-6-phenyl-2-pyrimidinylthio)acetic acid ethyl ester in 200 ml. of phosphorus oxychloride was heated under reflux for 17 hr. The excess phosphorus oxychloride was removed in a rotary evaporator. The residual oil crystallized on standing. Recrystallization from petroleum ether afforded 8.7 g of the title compound, mp. 82°-84°C.

Workup

  1. temperatureunder reflux for 17 hr
  2. customThe excess phosphorus oxychloride was removed in a rotary evaporator
  3. customThe residual oil crystallized
  4. customRecrystallization from petroleum ether

Sources & evidence

ORD record
ord-611a31bead49420092431181a5a85dca
Source dataset
uspto-grants-1976_02
Patent number
US03940394

Reaction notes

Loading…