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

HRID 1486260ノート

反応式

HRID 1486260 の反応式
[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]

参加物

4

反応物 1

HCID 86717927HCID 86717927、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-b9f407fbfb5e43e3bab34685d1cc59f6
出典データセット
uspto-grants-2016_08
特許番号
US09422285B2

反応ノート

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