Hydrazine hydrate (1:1) → 4-Hydrazinyl-6-(piperidin-1-yl)pyrimidine

HRID 37890노트

반응식

HRID 37890 반응식
O.[NH2:2][NH2:3].Cl[C:5]1[CH:10]=[C:9]([N:11]2[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]2)[N:8]=[CH:7][N:6]=1>C(O)C>[NH:2]([C:5]1[CH:10]=[C:9]([N:11]2[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]2)[N:8]=[CH:7][N:6]=1)[NH2:3]

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 5978704-Chloro-6-piperidin-1-ylpyrimidine

생성물 1

HCID 441403054-Hydrazinyl-6-(piperidin-1-yl)pyrimidine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

With stirring and at RT, 17.7 ml (18.2 g, 364.2 mmol) of hydrazine hydrate are added dropwise to a solution of 6.0 g (30.4 mmol) of 4-chloro-6-piperidin-1-ylpyrimidine in 50 ml of ethanol. The reaction solution is stirred at 80° C. for a further 16 h. For work-up, the mixture is concentrated under reduced pressure, the residue is stirred in water, the precipitated solid is filtered off, the filter residue is washed twice with in each case 150 ml of water and twice with in each case 100 ml of diethyl ether and the product is dried under reduced pressure.

후처리

  1. stirringThe reaction solution is stirred at 80° C. for a further 16 h
  2. concentrationFor work-up, the mixture is concentrated under reduced pressure
  3. stirringthe residue is stirred in water
  4. filtrationthe precipitated solid is filtered off
  5. washthe filter residue is washed twice with in each case 150 ml of water and twice with in each case 100 ml of diethyl ether
  6. customthe product is dried under reduced pressure

출처 및 근거

ORD 기록
ord-64a84a97abe3476381b6b4865a6319a0
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524699B2

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