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

HRID 876660노트

반응식

HRID 876660 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-9b36ff42a00c4e619d950cb2e8641dfe
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08987261B2

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