Triethylamine → 5-Amino-1-cyclohexyl-1H-pyrazole-4-carbonitrile

HRID 400489

반응식

HRID 400489 반응식
C(O[CH:4]=[C:5]([C:8]#[N:9])[C:6]#[N:7])C.C(N(CC)CC)C.Cl.[CH:18]1([NH:24][NH2:25])[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1>C(O)C>[NH2:9][C:8]1[N:24]([CH:18]2[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]2)[N:25]=[CH:4][C:5]=1[C:6]#[N:7]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 671522-(Ethoxymethylene)propanedinitrileHCID 207836Cyclohexylhydrazine hydrochloride

생성물 1

HCID 6900055-Amino-1-cyclohexyl-1H-pyrazole-4-carbonitrile

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

First ethoxymethylenemalononitrile (2.43 g, 19.9 mmol) and then 8 ml of triethylamine are added to a solution of cyclohexylhydrazine hydrochloride (3 g, 19.9 mmol) in 36 ml of ethanol at room temperature. The mixture is refluxed for 20 min and then cooled. The solvent is stripped off in a rotary evaporator, and the residue is taken up in DCM, washed with aqueous sodium bicarbonate solution, dried over sodium sulfate, filtered and concentrated in vacuo. The crude product is chromatographed on silica gel (mobile phase: dichloromethane/methanol 0-10%).

후처리

  1. temperatureThe mixture is refluxed for 20 min
  2. temperaturecooled
  3. customThe solvent is stripped off in a rotary evaporator
  4. washwashed with aqueous sodium bicarbonate solution
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe crude product is chromatographed on silica gel (mobile phase: dichloromethane/methanol 0-10%)

출처 및 근거

ORD 기록
ord-b8b80f04833748f58fbc7a0ade4d0bef
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08741907B2

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