Hydrazine hydrate (1:1) → HCID 20325484, compound

HRID 838975Notes

Reaction equation

HRID 838975 reaction equation
[C:1]([NH:5][CH2:6][CH:7]([OH:21])[CH2:8][O:9][C:10]1[CH:19]=[CH:18][CH:17]=[C:16]2[C:11]=1[CH:12]=[N:13][NH:14][C:15]2=S)([CH3:4])([CH3:3])[CH3:2].O.[NH2:23][NH2:24]>C(O)C>[C:1]([NH:5][CH2:6][CH:7]([OH:21])[CH2:8][O:9][C:10]1[CH:19]=[CH:18][CH:17]=[C:16]2[C:11]=1[CH:12]=[N:13][N:14]=[C:15]2[NH:23][NH2:24])([CH3:4])([CH3:3])[CH3:2]

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 20325510HCID 20325510, compound

Product 1

HCID 20325484HCID 20325484, compoundYield 100%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A stirred mixture of 5-(3-t-butylamino-2-hydroxypropoxy)-1(2H)-phthalazinthione (0.5 g), ethanol (50 ml) and hydrazine hydrate (15 ml) was heated under reflux for 21 hours. Ethanol and excess of hydrazine were removed by evaporation under reduced pressure to give 5-(3-t-butylamino-2-hydroxypropoxy)-1-hydrazinophthalazine (0.5 g, 100%) which was treated with 1.0N sulphuric acid (3.26 ml). Evaporation under reduced pressure gave the crude salt which was crystallised from aqueous methanol to give 5-(3-t-butylamino-2-hydroxypropoxy)-1-hydrazinophthalazine sulphate hydrate (0.45 g, 65%, m.p. 274°-276°, decomposition).

Workup

  1. temperaturewas heated
  2. temperatureunder reflux for 21 hours
  3. customEthanol and excess of hydrazine were removed by evaporation under reduced pressure

Sources & evidence

ORD record
ord-1da6c13f3a104f1f8a32cd923614b01a
Source dataset
uspto-grants-1978_06
Patent number
US04093725

Reaction notes

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