Phosphorus oxychloride → HCID 21272369, compound

HRID 1193520Notes

Reaction equation

HRID 1193520 reaction equation
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([NH:9][CH:10]2[NH:14][N:13]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[C:12](=O)[CH2:11]2)=[CH:5][CH:4]=1.P(Cl)(Cl)([Cl:24])=O>O>[Cl:24][C:11]1[C:10]([NH:9][C:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)=[N:14][N:13]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:12]=1

Participants

4

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 21272308HCID 21272308, compound

Product 1

HCID 21272369HCID 21272369, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A mixture of 5-(4-methoxyphenylamino)-2-phenylpyrazolidin-3-one (2.81 g) and excess phosphorous oxychloride (4 ml) was heated on a steam bath at 100° for 1 hour. Water was added and the aqueous phase extracted with dichloromethane. The organic phase was dried over magnesium sulphate, filtered and evaporated to dryness, and the title compound was obtained as a colourless solid (1.5 g), mp 119°-121° by recrystallisation from cyclohexane.

Workup

  1. temperaturewas heated on a steam bath at 100° for 1 hour
  2. extractionthe aqueous phase extracted with dichloromethane
  3. dry with materialThe organic phase was dried over magnesium sulphate
  4. filtrationfiltered
  5. customevaporated to dryness

Sources & evidence

ORD record
ord-b77d94730efc4b23ae0b1eec3662c61a
Source dataset
uspto-grants-1989_03
Patent number
US04810719

Reaction notes

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