2'-Chloro-4'-fluoro-5'-nitroacetanilide → 5'-Amino-2'-chloro-4'-fluoroacetanilide

HRID 380797ノート

反応式

HRID 380797 の反応式
[Cl:1][C:2]1[CH:11]=[C:10]([F:12])[C:9]([N+:13]([O-])=O)=[CH:8][C:3]=1[NH:4][C:5](=[O:7])[CH3:6]>[Pt].O1CCCC1.C(OCC)(=O)C.C(O)C>[NH2:13][C:9]1[C:10]([F:12])=[CH:11][C:2]([Cl:1])=[C:3]([CH:8]=1)[NH:4][C:5](=[O:7])[CH3:6]

参加物

4

反応物 1

HCID 183659292'-Chloro-4'-fluoro-5'-nitroacetanilide

生成物 1

HCID 183659355'-Amino-2'-chloro-4'-fluoroacetanilide

試薬・触媒・溶媒 2

HCID 23939Platinum触媒HCID 18365940Tetrahydrofuran ethyl acetate ethanol溶媒

実験手順

A mixture of 2′-chloro-4′-fluoro-5′-nitroacetanilide (26.1 g, 112 mmol) and 5% platinum on carbon (7.8 g, 30 wt %) in a tetrahydrofuran/ethyl acetate/ethanol solution (1:1:1) is hydrogenated at 50 psi for 22 hours and filtered. The resultant filtrate is concentrated in vacuo to obtain a solid which is recrystallized from an ethanol/water solution to give the title product as off-white plates (14.5 g, mp 176-178° C.).

後処理

  1. filtrationfiltered
  2. concentrationThe resultant filtrate is concentrated in vacuo
  3. customto obtain a solid which
  4. customis recrystallized from an ethanol/water solution

出典と根拠

ORDレコード
ord-b903eb748ad94809a5f45a9ac72ee422
出典データセット
uspto-grants-2001_10
特許番号
US06303783B1

反応ノート

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