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

HRID 242247

반응식

HRID 242247 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 (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.

후처리

  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

출처 및 근거

ORD 기록
ord-b52930eea51e4977b80f10005dc45379
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08653111B2

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