Water → 3-(3-Chloropropyl)-5,5-dimethyl-2,4-imidazolidinedione
反応式
[CH3:1][C:2]1([CH3:9])[NH:6][C:5](=[O:7])[NH:4][C:3]1=[O:8].Br[CH2:11][CH2:12][CH2:13][Cl:14].C([O-])([O-])=O.[Cs+].[Cs+].O>CN(C=O)C>[Cl:14][CH2:13][CH2:12][CH2:11][N:4]1[C:3](=[O:8])[C:2]([CH3:9])([CH3:1])[NH:6][C:5]1=[O:7]参加物
6
実験手順
A mixture of 5,5-dimethylhydantoin (5.25 g), 1-bromo-3-chloropropane (8.5 mL), and Cs2CO3 (20.78 g) in 40 mL DMF was allowed to react overnight. The reaction was poured into 125 mL H2O, extracted with ether, and the combined extracts dried over MgSO4. The crude extract was filtered, then reduced in vacuo to yield a clear oil. The residue was chromatographed (50% EtOAc in hexanes) to yield 3-(3-chloropropyl)-5,5-dimethylimidazolidinedione as a white solid.
後処理
- customto react overnight
- extractionextracted with ether
- dry with materialthe combined extracts dried over MgSO4
- extractionThe crude extract
- filtrationwas filtered
- customto yield a clear oil
- customThe residue was chromatographed (50% EtOAc in hexanes)
出典と根拠
- ORDレコード
- ord-a2004397838f4978bd246b99427c8017
- 出典データセット
- uspto-grants-2006_10
- 特許番号
- US07125865B2
反応ノート
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