4-Nitrophenol → 4-Nitrophenyl 2-bromo-2-methylpropanoate
반응식
[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]참가 물질
5
실험 절차
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.
후처리
- temperaturecooled in an icebath
- filtrationthe solids were filtered off
- concentrationthe solution concentrated
- customrecrystallized from 100 ml methanol
출처 및 근거
- ORD 기록
- ord-93eb0c417ac942a6a9a3f2126e9f7437
- 출처 데이터셋
- uspto-grants-2009_12
- 특허 번호
- US07632875B2
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