Triethylamine → 2,2-Dimethyl-5-(pyrrolidin-2-ylidene)-1,3-dioxane-4,6-dione
반응식
CO[C:3]1[CH2:4][CH2:5][CH2:6][N:7]=1.[C:8]1(=[O:17])[O:16][C:13]([CH3:15])([CH3:14])[O:12][C:10](=[O:11])[CH2:9]1.C(N(CC)CC)C>C1C=CC=CC=1>[CH3:14][C:13]1([CH3:15])[O:16][C:8](=[O:17])[C:9](=[C:3]2[CH2:4][CH2:5][CH2:6][NH:7]2)[C:10](=[O:11])[O:12]1참가 물질
5
실험 절차
A solution of 5-Methoxy-3,4-dihydro-2H-pyrrole (5.35 g, 54.0 mmol), isopropylidene malonate (7.78 g, 54.0 mmol), triethylamine (1.35 mL, 9.7 mmol) and benzene (55 mL) is refluxed under nitrogen overnight. The reaction is cooled to RT and concentrated and the crude product is recrystalized from EtOH (95 mL) to give the title compound as a white solid (8.13 g, 38.5 mmol). 1H NMR (CDCl3, 300 MHz) 3.73(t, 2H), 3.35(t, 2H), 2.20-2.08(m, 2H), 1.66(s, 6H).
후처리
- concentrationconcentrated
- customthe crude product is recrystalized from EtOH (95 mL)
출처 및 근거
- ORD 기록
- ord-5e7deb17ac814ff1907339b9a7fbd611
- 출처 데이터셋
- uspto-grants-2008_04
- 특허 번호
- US07361663B2
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