Acetic Acid → HCID 53728512, compound

HRID 2413740Notes

Reaction equation

HRID 2413740 reaction equation
[CH3:1][N:2]([CH3:7])[C:3](=[S:6])[NH:4][NH2:5].[C:8]([C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([C:17](=O)[CH3:18])[N:12]=1)(=O)[CH3:9].C(O)(=O)C>CCO>[CH3:1][N:2]([CH3:7])[C:3](=[S:6])[NH:4][N:5]=[C:8]([C:11]1[N:12]=[C:13]([C:17](=[N:5][NH:4][C:3]([N:2]([CH3:7])[CH3:1])=[S:6])[CH3:18])[CH:14]=[CH:15][CH:16]=1)[CH3:9]

Participants

5

Reactant 3

HCID 176Acetic AcidHCID 707902,6-DiacetylpyridineHCID 27337004,4-Dimethyl-3-thiosemicarbazide

Product 1

HCID 53728512HCID 53728512, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A mixture of 4,4-dimethylthiosemicarbazide (2.70 g, 0.022 mol) and 2,6-diacetylpyridine (1.63 g, 0.10 mol) in 95% EtOH (45 ml) containing glacial acetic acid (0.5 ml) was heated by a steam bath for 1 h and 10 min and allowed to cool to ambient temperature. The yellow precipitate was collected by filtration, washed with 95% EtOH, and subsequently recrystallized from toluene: yield 2.72 g (73%); mp 215° (dec).

Workup

  1. temperaturewas heated by a steam bath for 1 h and 10 min
  2. filtrationThe yellow precipitate was collected by filtration
  3. washwashed with 95% EtOH
  4. customsubsequently recrystallized from toluene

Sources & evidence

ORD record
ord-a0af7a1eca7442dcac6efbdf88b9d9c5
Source dataset
uspto-grants-1988_01
Patent number
US04719221

Reaction notes

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