5-Nitro-2,3,4-trifluorobenzotrifluoride → HCID 15614237、化合物
反応式
[F:1][C:2]1[C:7]([F:8])=[C:6]([F:9])[C:5]([N+:10]([O-])=O)=[CH:4][C:3]=1[C:13]([F:16])([F:15])[F:14]>O1CCCC1.[Ni]>[F:1][C:2]1[C:7]([F:8])=[C:6]([F:9])[C:5]([NH2:10])=[CH:4][C:3]=1[C:13]([F:15])([F:16])[F:14]参加物
4
実験手順
35 g of 2,3,4-trifluoro-5-nitro-benzotrifluoride in 150 ml of tetrahydrofuran were initially introduced into a hydrogenation apparatus, 3 g of Raney nickel were added and, after flushing with nitrogen, the mixture was hydrogenated to constant pressure with 30 bar of hydrogen at 25° to 45° C. After completion of the hydrogen uptake, the pressure was released and the reaction solution was filtered and subsequently fractionally distilled. 27 g of 2,3,4-trifluoro-5-amino-benzotrifluoride were obtained with a boiling point of 82° to 83° C. at 15 mbar.
後処理
- additionwere added
- customafter flushing with nitrogen
- customwas hydrogenated to constant pressure with 30 bar of hydrogen at 25° to 45° C
- filtrationthe reaction solution was filtered
- distillationsubsequently fractionally distilled
出典と根拠
- ORDレコード
- ord-2cdd080e605843298aca1d905ea8d5da
- 出典データセット
- uspto-grants-1992_01
- 特許番号
- US05082971
反応ノート
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