L-Valine → 2,5-Oxazolidinedione, 4-(1-methylethyl)-, (4S)-
反応式
[C:1](Cl)(Cl)=[O:2].[NH2:5][C@H:6]([C:10]([OH:12])=[O:11])[CH:7]([CH3:9])[CH3:8]>C1(C)C=CC=CC=1.C1COCC1>[CH:7]([C@H:6]1[C:10](=[O:11])[O:12][C:1](=[O:2])[NH:5]1)([CH3:9])[CH3:8]参加物
5
反応条件
- 温度
- 55 °C
実験手順
30.4 ml (57.47 mmol, 1.08 eq.) of a 20% solution of phosgene in toluene were added slowly at r.t. to a stirred solution of 6.26 g (53.44 mmol) L-valine (81a) in 63 ml dry THF. After the complete addition the mixture was heated at 55° C. for 4 h. Then a stream of nitrogen was bubbled through the solution and passed after that through a 1M aq. NaOH-solution for 20 min. before the solvent was evaporated. Recrystallization of the obtained residue from PE/Ether (2:1) yielded 3.62 g (25.29 mmol, 47.32%) (S)-4-Isopropyl-oxazolidine-2,5-dione (86) as a white solid.
後処理
- additionAfter the complete addition the mixture
- customThen a stream of nitrogen was bubbled through the solution
- customfor 20 min.
- customwas evaporated
- customRecrystallization of the obtained residue from PE/Ether (2:1)
出典と根拠
- ORDレコード
- ord-337bcec8626d4d83b62caa489c1b37ab
- 出典データセット
- uspto-grants-2007_12
- 特許番号
- US07312246B2
反応ノート
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