Hydrazine hydrate (1:1) → (6-Morpholin-4-ylpyrimidin-4-yl)hydrazine

HRID 242247

Reaction equation

HRID 242247 reaction equation
Cl[C:2]1[N:7]=[CH:6][N:5]=[C:4]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)[CH:3]=1.O.[NH2:15][NH2:16]>C(O)C>[NH:15]([C:2]1[N:7]=[CH:6][N:5]=[C:4]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)[CH:3]=1)[NH2:16]

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 7960704-(6-Chloropyrimidin-4-yl)morpholine

Product 1

HCID 13393622(6-Morpholin-4-ylpyrimidin-4-yl)hydrazine

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

53.0 g (2.7 mmol) 4-(6-chloropyrimidin-4-yl)morpholine are initially introduced into 260 ml ethanol. 132.9 g (2.7 mol) hydrazine hydrate are added and the mixture is stirred under reflux for 16 h. Thereafter, it is cooled to RT and approx. half of the solvent is removed by distillation. The mixture is cooled to 0° C. and the solid formed is filtered off It is rinsed with cold ethanol and the solid is dried first in air and then in vacuo.

Workup

  1. temperatureunder reflux for 16 h
  2. customis removed by distillation
  3. temperatureThe mixture is cooled to 0° C.
  4. customthe solid formed
  5. filtrationis filtered off It
  6. washis rinsed with cold ethanol
  7. customthe solid is dried first in air

Sources & evidence

ORD record
ord-b52930eea51e4977b80f10005dc45379
Source dataset
uspto-grants-2014_02
Patent number
US08653111B2

Linked notes

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