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

HRID 876656노트

반응식

HRID 876656 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

반응 조건

온도
80 °C

실험 절차

17.7 ml (18.2 g, 364.2 mmol) hydrazine hydrate are added dropwise to a solution of 6.0 g (30.4 mmol) 4-chloro-6-piperidin-1-ylpyrimidine in 50 ml ethanol at RT, while stiffing. The reaction solution is subsequently stirred at 80° C. for 16 h. For working up, the mixture is concentrated in vacuo, the residue is stirred in water, the solid which has precipitated out is filtered off, the residue on the filter is washed twice with 150 ml water each time and twice with 100 ml diethyl ether each time and the product is dried in vacuo.

후처리

  1. concentrationthe mixture is concentrated in vacuo
  2. stirringthe residue is stirred in water
  3. customthe solid which has precipitated out
  4. filtrationis filtered off
  5. washthe residue on the filter is washed twice with 150 ml water each time
  6. dry with materialtwice with 100 ml diethyl ether each time and the product is dried in vacuo

출처 및 근거

ORD 기록
ord-3a09ba6981e249eca5b56922820a7c3a
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08987261B2

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