Hydrazine hydrate (1:1) → HCID 34176375, compound

HRID 1863934Notes

Reaction equation

HRID 1863934 reaction equation
Cl[C:2]1[N:7]2[N:8]=[CH:9][N:10]=[C:6]2[CH:5]=[CH:4][N:3]=1.O.[NH2:12][NH2:13]>C(O)C>[NH:12]([C:2]1[N:7]2[N:8]=[CH:9][N:10]=[C:6]2[CH:5]=[CH:4][N:3]=1)[NH2:13]

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 126038175-Chloro[1,2,4]triazolo[1,5-c]pyrimidine

Product 1

HCID 34176375HCID 34176375, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent2×

Procedure

A solution of 155 mg (1 mmol) of 5-chloro[1,2,4]triazolo[1,5-c]pyrimidine [D. J. Brown and K. Shinozuka, Aust. J. Chem., 33, 1147 (1980)] in 6 mL of dry ethanol was added gradually to a vigorously stirred solution of 198 mg (204 mg, 4 mmol) of hydrazine monohydrate in 2 mL of dry ethanol. A white precipitate separated during the addition. After 1.5 h, the solid was collected on a filter. It was suspended in 2 mL of concentrated ammonium hydroxide and agitated for a few minutes. The solid was then collected on a filter and washed with some additional concentrated ammonium hydroxide, then with some ethanol, and finally with a large volume of diethyl ether. After drying, the title compound was obtained as a white solid, mp 245-246° C. (decomposition). LC-MS 151 (M+1).

Workup

  1. customA white precipitate separated during the addition
  2. customthe solid was collected on a filter
  3. customThe solid was then collected on
  4. filtrationa filter
  5. washwashed with some additional concentrated ammonium hydroxide
  6. customAfter drying

Sources & evidence

ORD record
ord-7c66aa33cfc743a6a46ae284730bdea5
Source dataset
uspto-grants-2009_12
Patent number
US07625888B2

Reaction notes

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