Benzyl Chloride → (R)-1-Benzyl-3-methylpiperazine

HRID 1951738노트

반응식

HRID 1951738 반응식
[CH3:1][C@@H:2]1[CH2:7][NH:6][CH2:5][CH2:4][NH:3]1.[CH2:8](Cl)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.C(=O)([O-])[O-].[K+].[K+]>C(O)C.[OH-].[Na+]>[CH2:8]([N:6]1[CH2:5][CH2:4][NH:3][C@H:2]([CH3:1])[CH2:7]1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

참가 물질

6

반응물 3

HCID 7503Benzyl ChlorideHCID 11430Potassium CarbonateHCID 73304342-Methylpiperazine, (R)-

생성물 1

HCID 6923226(R)-1-Benzyl-3-methylpiperazine수율 49%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 14798Sodium Hydroxide용매

실험 절차

A mixture of 1.0 g (10 mmol) (R)-2-methylpiperazine, 1.3 g (10 mmol) benzyl chloride and 4.1 g (30 mmol) potassium carbonate in 10 ml ethanol was heated at reflux over night. After cooling to room temperature the reaction mixture was diluted with a 0.5 M aqueous solution of sodium hydroxide and extracted with three portions of dichloromethane. The combined organic extracts were dried over sodium sulfate and concentrated. Flash column chromatography gave 0.93 g (49%) of the title compound as an off-white solid. MS m/e (%): 191 (M+H+, 100)

후처리

  1. temperaturewas heated
  2. temperatureat reflux over night
  3. extractionextracted with three portions of dichloromethane
  4. dry with materialThe combined organic extracts were dried over sodium sulfate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-bb47dae0217b480a83c0b6e5ccfe3434
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08404708B2

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