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

HRID 37892

반응식

HRID 37892 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7c389d41bf3a4ef4b3baa8420d5e64df
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524699B2

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