Hydrazine hydrate (1:1) → HCID 15289682, compound

HRID 37507Notes

Reaction equation

HRID 37507 reaction equation
[NH2:1][C:2]1[C:3]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)=[N:4][C:5]([S:18]([C:21]2[CH:26]=[CH:25][C:24]([CH3:27])=[CH:23][CH:22]=2)(=[O:20])=[O:19])=[C:6]([C:13]([O:15]CC)=O)[C:7]=1[C:8]([O:10]CC)=O.O.[NH2:35][NH2:36]>C(O)C>[NH2:1][C:2]1[C:7]2[C:8](=[O:10])[NH:36][NH:35][C:13](=[O:15])[C:6]=2[C:5]([S:18]([C:21]2[CH:22]=[CH:23][C:24]([CH3:27])=[CH:25][CH:26]=2)(=[O:19])=[O:20])=[N:4][C:3]=1[C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=1

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 15289703HCID 15289703, compound

Product 1

HCID 15289682HCID 15289682, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent2×

Conditions

Temperature
90 °C

Procedure

To 0.251 g of 3-amino-4,5-diethoxycarbonyl-2-phenyl-6-(p-tolylsulfonyl)pyridine were added 2 ml of hydrazine monohydrate and 2 ml of ethanol, and the mixture was stirred at 90° C. for 2 hours. After ethanol was added, the mixture was cooled. The resulting precipitate was collected by filtration and washed with ethanol. The thus obtained precipitate was suspended in 30 ml of water, and 2 ml of acetic acid was added thereto. After the mixture was heated, it was cooled. The resulting precipitate was collected by filtration, washed with water and dried to give 0.15 g of the title compound.

Workup

  1. temperaturethe mixture was cooled
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed with ethanol
  4. addition2 ml of acetic acid was added
  5. temperatureAfter the mixture was heated
  6. temperatureit was cooled
  7. filtrationThe resulting precipitate was collected by filtration
  8. washwashed with water
  9. customdried

Sources & evidence

ORD record
ord-b02405f4b5644b56aece380d4c1da0a1
Source dataset
uspto-grants-1995_05
Patent number
US05420275

Reaction notes

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