반응식
[N+:1]([O-:4])(O)=[O:2].NC(N)=O.[CH3:9][C:10]1([CH3:20])[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:12](=[O:19])[CH2:11]1>>[CH3:9][C:10]1([CH3:20])[C:18]2[C:13](=[CH:14][C:15]([N+:1]([O-:4])=[O:2])=[CH:16][CH:17]=2)[C:12](=[O:19])[CH2:11]1참가 물질
4
반응 조건
- 온도
- -10 °C
실험 절차
A mixture of nitric acid (90% fuming, 35 mL) and urea (0.17 g) was cooled to -10° C. and purged with air for 20 minutes; 3,3-dimethyl-1-indanone (8.68 g, 54.2 mmoles) was added and the reaction was stirred for two hours at -10° C. to 5° C. The reaction mixture was poured into ice/H2O and extracted with ethyl acetate. The combined extracts were washed with distilled H2O, saturated NaHCO3 solution, saturated NaCl solution, and dried over MgSO4. The solvent was recovered under vacuum to obtain 10.0 g of a yellow solid. The crude product was recrystallized from methanol in two crops to obtain 8.08 g (71%) of the title D compound as yellow needles. MS: M- @ 205.
후처리
- custompurged with air for 20 minutes
- extractionextracted with ethyl acetate
- washThe combined extracts were washed with distilled H2O, saturated NaHCO3 solution, saturated NaCl solution
- dry with materialdried over MgSO4
- customThe solvent was recovered under vacuum
출처 및 근거
- ORD 기록
- ord-bff1c78e3d7947c5968302598b186785
- 출처 데이터셋
- uspto-grants-1996_05
- 특허 번호
- US05514690
연결된 노트
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