Hydrazine hydrate (1:1) → HCID 20484846, compound

HRID 648082Notes

Reaction equation

HRID 648082 reaction equation
[OH:1][C:2]([CH3:16])([CH3:15])[CH2:3][C:4](=O)[C:5](=[C:11]([CH3:13])[CH3:12])[C:6]([O:8][CH2:9][CH3:10])=[O:7].O.[NH2:18][NH2:19]>C(O)(=O)C>[CH3:12][C:11]1([CH3:13])[NH:19][N:18]=[C:4]([CH2:3][C:2]([OH:1])([CH3:16])[CH3:15])[CH:5]1[C:6]([O:8][CH2:9][CH3:10])=[O:7]

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 20484848HCID 20484848, compound

Product 1

HCID 20484846HCID 20484846, compoundYield 98%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Conditions

Temperature
180 °C

Procedure

500 mg of the product of Step B were added to 3 ml of acetic acid and 121 mg of hydrazine hydrate and the temperature rose spontaneously to 40° C. The acetic acid was distilled by heating the mixture up to 180° C. during which the majority of the acetic acid was removed. The mixture was cooled and water was added thereto. The mixture was extracted with chloroform and the organic phase was dried over magnesium sulfate and evaporated to dryness to obtain 520 mg of ethyl 4,5-dihydro-5,5-dimethyl-3-(2-hydroxy-2-methylpropyl)-[1H]-pyrazole-4-carboxylate in the form of a liquid.

Workup

  1. customrose spontaneously to 40° C
  2. distillationThe acetic acid was distilled
  3. customwas removed
  4. temperatureThe mixture was cooled
  5. additionwater was added
  6. extractionThe mixture was extracted with chloroform
  7. dry with materialthe organic phase was dried over magnesium sulfate
  8. customevaporated to dryness

Sources & evidence

ORD record
ord-d2d3754e1e0f45e2a8e2ce7870b7241a
Source dataset
uspto-grants-1983_10
Patent number
US04410721

Reaction notes

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