(E)-3-(3-Fluoro-4-nitro-phenyl)-acrylic acid tert-butyl ester → Tert-butyl 3-(4-amino-3-fluorophenyl)propanoate

HRID 1690563ノート

反応式

HRID 1690563 の反応式
[C:1]([O:5][C:6](=[O:19])/[CH:7]=[CH:8]/[C:9]1[CH:14]=[CH:13][C:12]([N+:15]([O-])=O)=[C:11]([F:18])[CH:10]=1)([CH3:4])([CH3:3])[CH3:2]>C(OCC)(=O)C.[Pd]>[C:1]([O:5][C:6](=[O:19])[CH2:7][CH2:8][C:9]1[CH:14]=[CH:13][C:12]([NH2:15])=[C:11]([F:18])[CH:10]=1)([CH3:4])([CH3:2])[CH3:3]

参加物

4

反応物 1

HCID 66905416(E)-3-(3-Fluoro-4-nitro-phenyl)-acrylic acid tert-butyl ester

生成物 1

HCID 66905628Tert-butyl 3-(4-amino-3-fluorophenyl)propanoate収率 99.7%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of (E)-3-(3-fluoro-4-nitro-phenyl)-acrylic acid tert-butyl ester (804 mg, 3.01 mmol) in ethyl acetate (10 ml) was hydrogenated on 10% palladium on charcoal for 30 min at 1.5 bar. The suspension was filtered, the filter cake washed with ethyl acetate and the filtrate evaporated and dried under high vacuum to give the product as light brown solid (713 mg, 3 mmol; 99%). This material was pure enough for the next step. MS: m/e=240.0 [M+H+].

後処理

  1. filtrationThe suspension was filtered
  2. washthe filter cake washed with ethyl acetate
  3. customthe filtrate evaporated
  4. customdried under high vacuum

出典と根拠

ORDレコード
ord-3c71a5041dd4452a8fc0a6de315399a4
出典データセット
uspto-grants-2012_04
特許番号
US08153663B2

反応ノート

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