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

HRID 1786709ノート

反応式

HRID 1786709 の反応式
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]

参加物

5

反応物 2

HCID 516892Sodium BicarbonateHCID 27242022-Bromobenzylamine hydrochloride

生成物 1

HCID 70183002-Bromo-N-(tert-butoxycarbonyl)benzylamine収率 95%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-d8d8511fd6714c77bb469f6797f331c4
出典データセット
uspto-grants-2009_03
特許番号
US07507753B2

反応ノート

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