Sodium Bicarbonate → 2-Bromo-N-(tert-butoxycarbonyl)benzylamine

HRID 1786709노트

반응식

HRID 1786709 반응식
Cl.[Br:2][C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1[CH2:5][NH2:6].[C:11](=[O:14])(O)[O-:12].[Na+]>C(OCC)(=O)C.O>[C:4]([O:12][C:11](=[O:14])[NH:6][CH2:5][C:4]1[CH:7]=[CH:8][CH:9]=[CH:10][C:3]=1[Br:2])([CH3:7])([CH3:5])[CH3:3]

참가 물질

5

반응물 2

HCID 516892Sodium BicarbonateHCID 27242022-Bromobenzylamine hydrochloride

생성물 1

HCID 70183002-Bromo-N-(tert-butoxycarbonyl)benzylamine수율 95%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 2-bromobenzylamine hydrochloride (5.00 g) and di-tert-butoxycarbonyl (5.39 g) in ethyl acetate (30 ml) was added saturated sodium bicarbonate solution (30 ml), and stirred at room temperature for 16 hours. The obtained reaction mixture was diluted with water, and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried with magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography to give the title compound as a colorless liquid (6.48 g, 95%).

후처리

  1. customThe obtained reaction mixture
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried with magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-d8d8511fd6714c77bb469f6797f331c4
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07507753B2

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