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

HRID 2275852ノート

反応式

HRID 2275852 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

Under argon, 39 g (107.6 mmol) of tert-butyl {3,3,3-trifluoro-2-[(2-hydroxy-1-phenylethyl)amino]-2-methyl-propyl}carbamate Example 244A were initially charged in ethanol (700 ml), and 5.44 g (53.8 mmol) of palladium(II) hydroxide (20% on activated carbon, moistened with water about 60%) were added. The reaction mixture was hydrogenated at atmospheric pressure for 16 h. The mixture was then filtered through silica gel and concentrated. The residue was purified by silica gel chromatography (cyclohexane/ethyl acetate gradient: from 9/1 to 6/4). This gave 15.8 g (61% of theory) of the target compound.

後処理

  1. filtrationThe mixture was then filtered through silica gel
  2. concentrationconcentrated
  3. customThe residue was purified by silica gel chromatography (cyclohexane/ethyl acetate gradient: from 9/1 to 6/4)

出典と根拠

ORDレコード
ord-8272f8652a6b470885ea8c9e04a8e0be
出典データセット
uspto-grants-2015_09
特許番号
US09126998B2

反応ノート

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