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

HRID 37892

反応式

HRID 37892 の反応式
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]

参加物

4

実験手順

53.0 g (0.27 mol) of 4-(6-chloropyrimidin-4-yl)morpholine are initially charged in 260 ml of ethanol. 132.9 g (2.7 mol) of hydrazine hydrate are added, and the mixture is stirred under reflux for 16 h. The mixture is cooled to RT, and half of the solvent is removed by distillation. The mixture is then cooled to 0° C., and the solid formed is filtered off. The solid is washed with cold ethanol and initially air-dried and then dried under reduced pressure.

後処理

  1. temperatureunder reflux for 16 h
  2. customhalf of the solvent is removed by distillation
  3. temperatureThe mixture is then cooled to 0° C.
  4. customthe solid formed
  5. filtrationis filtered off
  6. washThe solid is washed with cold ethanol
  7. custominitially air-dried
  8. customdried under reduced pressure

出典と根拠

ORDレコード
ord-7c389d41bf3a4ef4b3baa8420d5e64df
出典データセット
uspto-grants-2013_09
特許番号
US08524699B2

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