Benzoyl Peroxide → ethyl (2E)-4-bromo-3-methylbut-2-enoate
反応式
[CH3:1][C:2]([CH3:9])=[CH:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].[Br:10]N1C(=O)CCC1=O.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C1C=CC=CC=1>[Br:10][CH2:1]/[C:2](/[CH3:9])=[CH:3]/[C:4]([O:6][CH2:7][CH3:8])=[O:5]参加物
5
実験手順
A mixture of ethyl 3,3-dimethylacrylate (12.8g, 100 mmol), N-bromosuccinimide (11.8g, 66 mmol), dry benzene (50 ml) and benzoyl peroxide (20 mg) was heated under reflux for 0.5h. After cooling, filtration, concentration and distillation, ethyl 4-bromo-3-methylcrotonate was obtained. The latter (33.8 mmol) was added dropwise to triethylphosphite (47.17 mmol) at 100°. The mixture was warmed to 150o and the residue purified by distillation to give triethyl 4-phosphono-3-methylcrotonate (b.p. 120° at 0.5 mm.Hg) as a cis/trans mixture.
後処理
- temperaturewas heated
- temperatureunder reflux for 0.5h
- temperatureAfter cooling
- filtrationfiltration, concentration and distillation
出典と根拠
- ORDレコード
- ord-e9742e99a8f04a57b372f8fea82a5f85
- 出典データセット
- uspto-grants-1992_11
- 特許番号
- US05162367
反応ノート
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