Chloroform → HCID 86709464、化合物
反応式
[C:1]([CH:4]([CH:10]([CH3:12])[CH3:11])[C:5]([O:7][CH2:8][CH3:9])=[O:6])(=[O:3])[CH3:2].[Br:13]Br.C(Cl)(Cl)Cl.C(OCC)(=O)C>O>[Br:13][CH2:2][C:1](=[O:3])[CH:4]([CH:10]([CH3:11])[CH3:12])[C:5]([O:7][CH2:8][CH3:9])=[O:6]参加物
6
実験手順
To a solution of ethyl 2-acetyl-3-methylbutanoate (5.10 g, 29.6 mmol) in water (10 mL) at 0° C. was added bromine (1.53 mL, 29.6 mmol) dropwise over 2 h. Chloroform (30 mL) was added and the resulting solution was stirred at rt for 16 h. Ethyl acetate (300 mL) was added to the reaction solution and the organic phase was dried over sodium sulfate and concentrated to give the title compound. 1HNMR (500 MHz, CDCl3), δ4.300-4.282 (m, 2H), 2.601-2.575 (m, 1H), 2.406 (s, 2H), 1.331-1.303 (t, J=7.1 Hz, 3H), 1.085-1.072 (d, J=6.5 Hz, 3H), 1.048-1.035 (d, J=6.7 Hz, 3H).
後処理
- dry with materialthe organic phase was dried over sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-6fa7b8a83b7342798482a610fb357dfe
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09206198B2
反応ノート
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