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

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

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

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

Sources & evidence

ORD record: ord-727693d69aa2469abc25a8ff25403163
Source dataset: uspto-grants-1995_05
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US05420275

Reaction notes

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