HCID 86717927, 화합물 → rac-tert-Butyl (2-amino-3,3,3-trifluoro-2-methylpropyl)carbamate

HRID 1486260노트

반응식

HRID 1486260 반응식
[F:1][C:2]([F:25])([F:24])[C:3]([NH:14]C(C1C=CC=CC=1)CO)([CH3:13])[CH2:4][NH:5][C:6](=[O:12])[O:7][C:8]([CH3:11])([CH3:10])[CH3:9]>C(O)C.[OH-].[Pd+2].[OH-]>[NH2:14][C:3]([CH3:13])([C:2]([F:1])([F:24])[F:25])[CH2:4][NH:5][C:6](=[O:12])[O:7][C:8]([CH3:11])([CH3:9])[CH3:10]

참가 물질

4

반응물 1

HCID 86717927HCID 86717927, 화합물

생성물 1

HCID 90136051rac-tert-Butyl (2-amino-3,3,3-trifluoro-2-methylpropyl)carbamate

시약·촉매·용매 2

HCID 9942167Palladium hydroxide촉매HCID 702Ethanol용매

실험 절차

39 g (107.6 mmol) of tert-butyl-{3,3,3-trifluoro-2-[(2-hydroxy-1-phenylethyl)amino]-2-methylpropyl}carbamate from Example 50A were initially charged under argon in ethanol (700 ml), and 5.44 g (53.8 mmol) of palladium(II) hydroxide (20% on activated carbon, water-moist, about 60%) were added. The reaction mixture was hydrogenated at standard pressure for 16 h. Then the reaction mixture was filtered through silica gel and concentrated. The residue was purified by means of silica gel chromatography (cyclohexane/ethyl acetate gradient: 9/1 to 6/4). This gave 15.8 g (61% of theory) of the target compound.

후처리

  1. filtrationThen the reaction mixture was filtered through silica gel
  2. concentrationconcentrated
  3. customThe residue was purified by means of silica gel chromatography (cyclohexane/ethyl acetate gradient: 9/1 to 6/4)

출처 및 근거

ORD 기록
ord-b9f407fbfb5e43e3bab34685d1cc59f6
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09422285B2

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