4-Nitrophenol → 4-Nitrophenyl 2-bromo-2-methylpropanoate
反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1)([O-:3])=[O:2].C(N(CC)CC)C.[Br:18][C:19]([CH3:24])([CH3:23])[C:20](Br)=[O:21]>O1CCCC1>[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([O:10][C:20](=[O:21])[C:19]([Br:18])([CH3:24])[CH3:23])=[CH:6][CH:5]=1)([O-:3])=[O:2]参加物
5
実験手順
4-Nitrophenol (8 gm, 56 mmol) in 100 ml anhydrous tetrahydrofuran was placed under a nitrogen atmosphere and cooled in an icebath. To this was added triethylamine (6.2 g, 61 mmol) followed by the dropwise addition of bromoisobutyryl bromide (14.1 g, 61 mmol) in 20 ml anhydrous tetrahydrofuran over 5 min. After stirring for 16 h, the solids were filtered off and the solution concentrated, and then recrystallized from 100 ml methanol to give 13.8 g yellow solid, >99% pure by HPLC.
後処理
- temperaturecooled in an icebath
- filtrationthe solids were filtered off
- concentrationthe solution concentrated
- customrecrystallized from 100 ml methanol
出典と根拠
- ORDレコード
- ord-93eb0c417ac942a6a9a3f2126e9f7437
- 出典データセット
- uspto-grants-2009_12
- 特許番号
- US07632875B2
反応ノート
読み込み中…