Hydrazine hydrate (1:1) → HCID 15289591, compound

HRID 37486Notes

Reaction equation

HRID 37486 reaction equation
[NH2:1][C:2]1[C:3]([CH3:18])=[N:4][CH:5]=[C:6]([C:13](OCC)=[O:14])[C:7]=1[C:8](OCC)=[O:9].O.[NH2:20][NH2:21]>>[NH2:1][C:2]1[C:7]2[C:8](=[O:9])[NH:21][NH:20][C:13](=[O:14])[C:6]=2[CH:5]=[N:4][C:3]=1[CH3:18]

Participants

3

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 15289695Diethyl 5-amino-6-methylpyridine-3,4-dicarboxylate

Product 1

HCID 15289591HCID 15289591, compound

Conditions

Temperature
100 °C

Procedure

To 57 mg of 3-amino-4,5-diethoxycarbonyl-2-methylpyridine was added 0.5 mL of hydrazine monohydrate, and the mixture was heated at 100° C. in a stream of nitrogen for 30 minutes. After the solvent was distilled off, the resulting crystals were collected by filtration with ethanol. Water was added to the crystals, and the mixture was neutralized with 1N hydrochloric acid, followed by collection of the crystals by filtration.

Workup

  1. distillationAfter the solvent was distilled off
  2. filtrationthe resulting crystals were collected by filtration with ethanol
  3. additionWater was added to the crystals
  4. filtrationfollowed by collection of the crystals by filtration

Sources & evidence

ORD record
ord-727693d69aa2469abc25a8ff25403163
Source dataset
uspto-grants-1995_05
Patent number
US05420275

Reaction notes

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