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

HRID 2275852노트

반응식

HRID 2275852 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

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-8272f8652a6b470885ea8c9e04a8e0be
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09126998B2

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