Water → HCID 136035444, compound

HRID 223702Notes

Reaction equation

HRID 223702 reaction equation
[C:1]([C:4]1[CH:5]=[C:6]2[C:11](=[C:12]([CH2:15][CH2:16][CH3:17])[C:13]=1[OH:14])[N:10]=[C:9]([C:18]([O:20][CH3:21])=[O:19])[CH2:8][C:7]2=O)(=[O:3])[CH3:2].P(Cl)(Cl)([Cl:25])=O.O>C1C=CC=CC=1>[C:1]([C:4]1[CH:5]=[C:6]2[C:11](=[C:12]([CH2:15][CH2:16][CH3:17])[C:13]=1[OH:14])[N:10]=[C:9]([C:18]([O:20][CH3:21])=[O:19])[CH:8]=[C:7]2[Cl:25])(=[O:3])[CH3:2]

Participants

5

Reactant 3

HCID 962WaterHCID 24813Phosphorus oxychlorideHCID 70472534HCID 70472534, compound

Product 1

HCID 136035444HCID 136035444, compound

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Procedure

The product of step (b) (3 g, 0.0099 mole) was dissolved in dry benzene (50 mls), treated with phosphoryl chloride (2.5 mls) and refluxed for 1 hour. The reaction mixture was cooled, poured into water and extracted with ether, which was then washed with water and dried over magnesium sulphate. The solvent was evaporated to leave 2.8 g of yellow-brown solid. Recrystallisation from cyclohexane gave yellow needles mp 163°-164°.

Workup

  1. temperaturerefluxed for 1 hour
  2. temperatureThe reaction mixture was cooled
  3. extractionextracted with ether, which
  4. washwas then washed with water
  5. dry with materialdried over magnesium sulphate
  6. customThe solvent was evaporated

Sources & evidence

ORD record
ord-f5d827f5e47d449ab80868670264d3aa
Source dataset
uspto-grants-1982_10
Patent number
US04356181

Reaction notes

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