1-Methylpiperazine → HCID 58447055, 화합물

HRID 1045741노트

반응식

HRID 1045741 반응식
Cl[C:2]1[CH:7]=[N:6][CH:5]=[C:4]([CH3:8])[N:3]=1.[CH3:9][N:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1>CCO>[CH3:8][C:4]1[CH:5]=[N:6][CH:7]=[C:2]([N:13]2[CH2:14][CH2:15][N:10]([CH3:9])[CH2:11][CH2:12]2)[N:3]=1

참가 물질

4

반응물 2

HCID 531671-MethylpiperazineHCID 71700952-Chloro-6-methylpyrazine

생성물 1

HCID 58447055HCID 58447055, 화합물수율 45.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A 250 mL round bottom flask was charged with 2-chloro-6-methylpyrazine (4.0 g, 0.031 mol), 1-methylpiperazine (12.4 g, 0.125 mol) and EtOH (100 mL). The resulting mixture was heated at reflux overnight. Work-up: the solvent was evaporated. The residue was mixed with saturated aqueous NaHCO3 (100 mL) and then extracted with CH2Cl2 (100 mL×3). The combined organic layers were dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was further purified by flash column chromatography on silica gel with 4% MeOH in CH2Cl2, to afford 2.7 g (45%) of the product as a white solid. MS m/z: 193 (M+H+).

후처리

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux overnight
  3. customthe solvent was evaporated
  4. additionThe residue was mixed with saturated aqueous NaHCO3 (100 mL)
  5. extractionextracted with CH2Cl2 (100 mL×3)
  6. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
  7. concentrationconcentrated in vacuo
  8. customThe residue was further purified by flash column chromatography on silica gel with 4% MeOH in CH2Cl2

출처 및 근거

ORD 기록
ord-0b741a4e7c41437fb51529d8cc3eea1f
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08569300B2

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