4-Fluorobenzyl chloride → (r)-1-(4-Fluorobenzyl)-3-methylpiperazine

HRID 11624

반응식

HRID 11624 반응식
[CH3:1][C@@H:2]1[CH2:7][NH:6][CH2:5][CH2:4][NH:3]1.[F:8][C:9]1[CH:16]=[CH:15][C:12]([CH2:13]Cl)=[CH:11][CH:10]=1.C(=O)([O-])O.[Na+]>C(O)C>[F:8][C:9]1[CH:16]=[CH:15][C:12]([CH2:13][N:6]2[CH2:5][CH2:4][NH:3][C@H:2]([CH3:1])[CH2:7]2)=[CH:11][CH:10]=1

참가 물질

5

반응물 3

HCID 96024-Fluorobenzyl chlorideHCID 516892Sodium BicarbonateHCID 73304342-Methylpiperazine, (R)-

생성물 1

HCID 11600914(r)-1-(4-Fluorobenzyl)-3-methylpiperazine수율 53.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of (2R)-2-methyl-piperizine (4.5 g, 45 mmol) in ethanol (80 mL) was added 4-fluorobenzyl chloride (5.38 mL, 45.0 mmol) and sodium hydrogen carbonate (11.3 g, 135 mmol). The reaction was refluxed overnight, cooled and concentrated. The remaining residue was diluted with dichloromethane and washed with water. The organic layer was separated and concentrated to give a clear oil. Chromatography on silica gel gave the title compound (5.0 g).

후처리

  1. temperatureThe reaction was refluxed overnight
  2. temperaturecooled
  3. concentrationconcentrated
  4. additionThe remaining residue was diluted with dichloromethane
  5. washwashed with water
  6. customThe organic layer was separated
  7. concentrationconcentrated
  8. customto give a clear oil

출처 및 근거

ORD 기록
ord-47c853a443844d0ebba44d6152144a8d
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07098212B2

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