5-(4-Fluorophenoxy)furan-2-carbaldehyde → C-(5-(4-Fluoro-phenoxy)-furan-2-yl)methylamine

HRID 2080148ノート

反応式

HRID 2080148 の反応式
[F:1][C:2]1[CH:15]=[CH:14][C:5]([O:6][C:7]2[O:11][C:10]([CH:12]=O)=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.[NH3:16].CO>[Ni]>[F:1][C:2]1[CH:15]=[CH:14][C:5]([O:6][C:7]2[O:11][C:10]([CH2:12][NH2:16])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 110419065-(4-Fluorophenoxy)furan-2-carbaldehydeHCID 21705897Ammonia methanol

生成物 1

HCID 23130578C-(5-(4-Fluoro-phenoxy)-furan-2-yl)methylamine収率 81%

試薬・触媒・溶媒 1

HCID 935Nickel触媒

実験手順

A suspension of 5-(4-fluoro-phenoxy)-furan-2-carbaldehyde described in Preparation Example 168 (4.3 g, 20.9 mmol), Raney nickel (1.5 g) and 7N ammonia-methanol solution (40 mL) was stirred at room temperature for 15 hours under hydrogen atmosphere (1 atm). The reaction solution was filtered through Celite pad to remove the catalyst, and the filtrate was concentrated. The residue was dissolved in ethyl acetate, filtered by NH silica gel lined over a glass filter, and then, this filtrate was concentrated to obtain the title compound (3.5 g, 16.9 mmol, 81%).

後処理

  1. filtrationThe reaction solution was filtered through Celite pad
  2. customto remove the catalyst
  3. concentrationthe filtrate was concentrated
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. filtrationfiltered by NH silica gel
  6. filtrationfilter
  7. concentrationthis filtrate was concentrated

出典と根拠

ORDレコード
ord-66a6a9f67f6d401a9c54654d1ef625cb
出典データセット
uspto-grants-2011_04
特許番号
US07932272B2

反応ノート

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