5-Fluoro-2-(2,2,2-trifluoroethoxy)nitrobenzene → 5-Fluoro-2-(2,2,2-trifluoroethoxy)aniline

HRID 2185920ノート

反応式

HRID 2185920 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]([O:11][CH2:12][C:13]([F:16])([F:15])[F:14])=[C:6]([N+:8]([O-])=O)[CH:7]=1>C(OCC)(=O)C.[Ni]>[F:1][C:2]1[CH:3]=[CH:4][C:5]([O:11][CH2:12][C:13]([F:14])([F:15])[F:16])=[C:6]([CH:7]=1)[NH2:8]

参加物

4

反応物 1

HCID 234479215-Fluoro-2-(2,2,2-trifluoroethoxy)nitrobenzene

生成物 1

HCID 174854135-Fluoro-2-(2,2,2-trifluoroethoxy)aniline収率 90.6%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
22.5 °C

実験手順

A mixture of 0.66 g of Compound 8A and 0.07 g of Raney-Nickel in 20 mL of ethyl acetate was stirred for 14 hours at 20-25° C. The catalyst was filtered off. The mixture was diluted with water. The organic layer was separated and the mixture extracted with 2×40 mL of ethyl acetate. The combined organic layers were washed with 20 mL of brine, dried over sodium sulphate and evaporated to dryness in vacuo to afford 0.52 g (90.6%) of Compound 8B as an oil.

後処理

  1. filtrationThe catalyst was filtered off
  2. additionThe mixture was diluted with water
  3. customThe organic layer was separated
  4. extractionthe mixture extracted with 2×40 mL of ethyl acetate
  5. washThe combined organic layers were washed with 20 mL of brine
  6. dry with materialdried over sodium sulphate
  7. customevaporated to dryness in vacuo

出典と根拠

ORDレコード
ord-e59feff57bef42659ba9126a19a4b812
出典データセット
uspto-grants-2002_06
特許番号
US06403594B1

反応ノート

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