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Water → HCID 178426271, compound

HRID 2085357
Notes
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Reaction equation

HRID 2085357 reaction equation
P(Cl)(Cl)(Cl)=O.[CH3:6][C:7]1[CH:8]=[C:9]([N:14]2[C:18](=[O:19])[CH:17]=[C:16]([CH3:20])[NH:15]2)[CH:10]=[CH:11][C:12]=1[CH3:13].O.CN(C)[CH:24]=[O:25]>>[CH3:6][C:7]1[CH:8]=[C:9]([N:14]2[C:18]([OH:19])=[C:17]([CH:24]=[O:25])[C:16]([CH3:20])=[N:15]2)[CH:10]=[CH:11][C:12]=1[CH3:13]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 4

HCID 962WaterHCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 117358291-(3,4-Dimethylphenyl)-3-methyl-3-pyrazolin-5-one

Product 1

HCID 178426271HCID 178426271, compoundYield 79%

Conditions

Temperature
100 °C

Procedure

Phosphorus oxychloride (4.82 mL, 51.6 mmol) was added dropwise to an ice-cooled, stirred suspension of 1-(3,4-dimethylphenyl)-3-methyl-3-pyrazolin-5-one (8.70 g, 43.0 mmol) in dimethylformamide (18.0 mL) at such a rate as to maintain the temperature below 20° C. After the addition, the mixture was heated at 100° C. for 2 h, then cooled, poured into iced water (200 mL). The resulting mixture was stirred for 18 h, then filtered. The solid was washed with water and dried to give the title compound (7.83 g, 79%) as a cream-coloured powder. MS (ES) m/e 231 [M+H]+.

Workup

  1. temperaturecooled
  2. temperatureto maintain the temperature below 20° C
  3. additionAfter the addition
  4. temperaturecooled
  5. stirringThe resulting mixture was stirred for 18 h
  6. filtrationfiltered
  7. washThe solid was washed with water
  8. customdried

Sources & evidence

ORD record
ord-9285bf0773724f04a9033744f88e9f7e
Source dataset
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06720345B1

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes