Water → HCID 54474705, 화합물

HRID 1038558노트

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HRID 1038558 반응식
[CH2:1]([N:8]1[CH2:13][C@H:12]([CH3:14])[NH:11][CH2:10][C@H:9]1[CH3:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CN(C)C.[C:20]([O:24][C:25](=O)[O:26]C(C)(C)C)([CH3:23])([CH3:22])[CH3:21].O>O1CCCC1>[CH2:1]([N:8]1[C@@H:9]([CH3:15])[CH2:10][N:11]([C:25]([O:24][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:26])[C@H:12]([CH3:14])[CH2:13]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 1146TrimethylamineHCID 10219638Carbonic acid, bis(1,1-dimethylethyl) esterHCID 10632028(2R,5S)-1-benzyl-2,5-dimethylpiperazine

생성물 1

HCID 54474705HCID 54474705, 화합물수율 60.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of (2R,5S)-1-benzyl-2,5-dimethylpiperazine (3.52 g, 17.2 mmol) in tetrahydrofuran (50 mL), trimethylamine (2.12 g, 20.9 mmol) and di-tert-butylcarbonate (4.56 g, 20.9 mmol) were added under ice-cold conditions, and the mixture was stirred for 15 minutes. Then, the mixture was stirred at room temperature for 5.5 hours. The reaction solution was added water, extracted with ethyl acetate, washed with brine, dried over sodium sulfate, and concentrated in vacuo. The obtained residue was purified by silica-gel column chromatography (hexane/ethyl acetate), and the title compound (3.16 g, 60%) was obtained as a pale yellow oil.

후처리

  1. stirringThen, the mixture was stirred at room temperature for 5.5 hours
  2. extractionextracted with ethyl acetate
  3. washwashed with brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe obtained residue was purified by silica-gel column chromatography (hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-fbe5005b02a4492ab1f8a3ec964f245f
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08551985B2

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