Ethanol → 1-(6-Hydrazinopyrimidin-4-yl)azetidin-3-ol

HRID 242241노트

반응식

HRID 242241 반응식
Cl[C:2]1[N:7]=[CH:6][N:5]=[C:4]([N:8]2[CH2:11][CH:10]([OH:12])[CH2:9]2)[CH:3]=1.O.[NH2:14][NH2:15].C(O)C>C1COCC1>[NH:14]([C:2]1[N:7]=[CH:6][N:5]=[C:4]([N:8]2[CH2:11][CH:10]([OH:12])[CH2:9]2)[CH:3]=1)[NH2:15]

참가 물질

5

반응물 3

HCID 702EthanolHCID 24654Hydrazine hydrate (1:1)HCID 579250791-(6-Chloropyrimidin-4-yl)azetidin-3-ol

생성물 1

HCID 552790421-(6-Hydrazinopyrimidin-4-yl)azetidin-3-ol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

960 mg (5.2 mmol) 1-(6-chloropyrimidin-4-yl)azetidin-3-ol and 2.5 ml (51.7 mmol) hydrazine hydrate are initially introduced into a mixture of 10 ml ethanol and 10 ml THF. The reaction is carried out at 130° C. for 1 h in a single mode microwave (CEM Explorer). The mixture is concentrated to approx. 20-50% of the original volume of liquid and is left to stand at RT for 48 h. The supernatant is decanted off from the solid formed and the solid is washed three times with 1.5 ml cold ethanol each time. It is dried under a high vacuum.

후처리

  1. concentrationThe mixture is concentrated to approx. 20-50% of the original volume of liquid
  2. waitis left
  3. waitto stand at RT for 48 h
  4. customThe supernatant is decanted off from the solid
  5. customformed
  6. washthe solid is washed three times with 1.5 ml cold ethanol each time
  7. customIt is dried under a high vacuum

출처 및 근거

ORD 기록
ord-74284d8763534535827587612fc912d9
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08653111B2

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