反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([Cl:10])=[CH:6][C:5]=1[OH:11])([O-])=O>C(O)C>[NH2:1][C:4]1[CH:9]=[CH:8][C:7]([Cl:10])=[CH:6][C:5]=1[OH:11]参加物
3
実験手順
To a solution of 2-nitro-5-chloro-phenol (2.2 g, 14.0 mmol) in ethanol (40 mL) was added PtS2-C (5%, 200 mg) and hydrogenated at 45 psi for 4 hours. The mixture was filtered through celite and washed with ethyl acetate (100 mL). The solvent was evaporated and purified by chromatography ((ethyl acetate-hexanes: 2-3) to afford 1.89 g (95%) of a light brown solid. Recrystallization afforded an analytical sample: mp 149-151° C.
後処理
- filtrationThe mixture was filtered through celite
- washwashed with ethyl acetate (100 mL)
- customThe solvent was evaporated
- custompurified by chromatography ((ethyl acetate-hexanes: 2-3)
出典と根拠
- ORDレコード
- ord-6d1c18612c75469ba512897708e8220a
- 出典データセット
- uspto-grants-2001_11
- 特許番号
- US06313114B1
関連ノート
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