Methanol → HCID 136332165, compound

HRID 2290359Notes

Reaction equation

HRID 2290359 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[C:9](=[N:11][OH:12])[CH3:10])=[CH:4][CH:3]=1.[NH2:14][NH:15][C:16]([NH2:18])=[S:17].CO>C(O)(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[N:14][NH:15][C:16]([NH2:18])=[S:17])[C:9](=[N:11][OH:12])[CH3:10])=[CH:4][CH:3]=1

Participants

5

Reactant 3

HCID 887MethanolHCID 2723789ThiosemicarbazideHCID 639963656472-72-1

Product 1

HCID 136332165HCID 136332165, compoundYield 86.5%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

A mixture of 4'-chloro-2-hydroxyiminopropiophenone (252.3 g), thiosemicarbazide (151.3 g), methanol (650 ml) water (300 ml), and acetic acid (9 ml) was refluxed for 31 hours with stirring. After cooling, the resulting precipitates were collected by filtration, washed successively with methanol, water and methanol, and then dried to give 4'-chloro-2-hydroxyiminopropiophenone thiosemicarbazone (298.88 g).

Workup

  1. temperaturewas refluxed for 31 hours
  2. temperatureAfter cooling
  3. customthe resulting precipitates
  4. filtrationwere collected by filtration
  5. washwashed successively with methanol, water and methanol
  6. customdried

Sources & evidence

ORD record
ord-d460d2d077154021a548584d4355b394
Source dataset
uspto-grants-1986_10
Patent number
US04616014

Reaction notes

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