Hydrochloric Acid → 4-Tert-butyl-2-chloro-5-nitro-phenol
反応式
[OH-].[K+].C(=O)(OC)[O:4][C:5]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[C:8]([C:14]([CH3:17])([CH3:16])[CH3:15])=[CH:7][C:6]=1[Cl:18].Cl>CO>[C:14]([C:8]1[C:9]([N+:11]([O-:13])=[O:12])=[CH:10][C:5]([OH:4])=[C:6]([Cl:18])[CH:7]=1)([CH3:17])([CH3:15])[CH3:16]参加物
5
実験手順
Potassium hydroxide (10.1 g, 181 mmol) was added to 4-tert-butyl-2-chloro-5-nitrophenyl methyl carbonate (40.0 g, 139 mmol) in MeOH (100 mL). After 30 min, the reaction was acidified with 1N HCl and extracted with dichloromethane. The combined organic layers were combined, dried over Na2SO4 and concentrated under vacuum. The crude residue was purified by column chromatography (Pet. Ether/EtOAc, 30:1) to give 4-tert-butyl-2-chloro-5-nitro-phenol (23.0 g, 68% over 2 steps).
後処理
- extractionextracted with dichloromethane
- dry with materialdried over Na2SO4
- concentrationconcentrated under vacuum
- customThe crude residue was purified by column chromatography (Pet. Ether/EtOAc, 30:1)
出典と根拠
- ORDレコード
- ord-41d51ce9b5a24271896790c84e6fc174
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08829204B2
反応ノート
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