3,5-Difluoro-4-(2-phenyldiazenyl)phenol → 4-Amino-3,5-difluorophenol
反応式
[F:1][C:2]1[CH:3]=[C:4]([OH:17])[CH:5]=[C:6]([F:16])[C:7]=1[N:8]=NC1C=CC=CC=1>CO.[Pd]>[NH2:8][C:7]1[C:2]([F:1])=[CH:3][C:4]([OH:17])=[CH:5][C:6]=1[F:16]参加物
4
実験手順
20.4 g (0.09 mol) of 3,5-difluoro-4-(phenyldiazenyl)phenol from Example 1 and 0.5 g of Pd/C (10%) were initially charged in 120 ml of methanol. The solution was degassed and aerated with hydrogen. The mixture was stirred at room temperature under a 1 bar hydrogen atmosphere for 16 hours. On completion of hydrogen uptake, the catalyst was filtered off and the filtrate concentrated on a rotary evaporator. The residue was chromatographed on silica gel (n-hexane/ethyl acetate, 3:1). The resulting solid was stirred with n-hexane and dried. 7.6 g (60%) of 4-amino-3,5-difluorophenol were obtained as a yellow-brown solid.
後処理
- customThe solution was degassed
- filtrationOn completion of hydrogen uptake, the catalyst was filtered off
- concentrationthe filtrate concentrated on a rotary evaporator
- customThe residue was chromatographed on silica gel (n-hexane/ethyl acetate, 3:1)
- stirringThe resulting solid was stirred with n-hexane
- customdried
出典と根拠
- ORDレコード
- ord-3541ad6a1a0e4a91b167c5b538f471c7
- 出典データセット
- uspto-grants-2008_04
- 特許番号
- US07358397B2
反応ノート
読み込み中…