4-Bromo-2-nitrobenzene-1-thiol → 2-Amino-4-bromobenzene-1-thiol
反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([SH:8])=[C:4]([N+:9]([O-])=O)[CH:3]=1.[H][H]>C1COCC1.[Ni]>[NH2:9][C:4]1[CH:3]=[C:2]([Br:1])[CH:7]=[CH:6][C:5]=1[SH:8]参加物
5
実験手順
The mixture of 4-bromo-2-nitro-benzenethiol and its disulfide from Example 2A (14.9 g, 53.5 mmol) in THF (450 mL) was mixed with Raney Ni (30 g, 100% wt). The mixture was hydrogenated in a 1000 mL Paar shaker at a hydrogen pressure of 40 psi at 50° C. for 41 hours. When the reaction was complete, the solids were filtered. The solid filter-cake was dissolved in pyridine (600 mL) at 100° C. and filtered to remove the Ni residue. This pyridine solution contained mostly the 2-amino-4-bromophenyldisulfide. Crude yield=11.9 g (92%)
後処理
- filtrationthe solids were filtered
- filtrationThe solid filter-cake
- dissolutionwas dissolved in pyridine (600 mL) at 100° C.
- filtrationfiltered
- customto remove the Ni residue
出典と根拠
- ORDレコード
- ord-047fe1c5f9834cbcb16b3e4e1a1cbfb3
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07094790B2
反応ノート
読み込み中…