Water → 3-(3-Chloropropyl)-5,5-dimethyl-2,4-imidazolidinedione
반응식
[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]참가 물질
6
실험 절차
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.
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-a2004397838f4978bd246b99427c8017
- 출처 데이터셋
- uspto-grants-2006_10
- 특허 번호
- US07125865B2
반응 노트
불러오는 중…