반응식
I[C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][C:10]([O:12][CH3:13])=[O:11])=[CH:4][CH:3]=1.[C:14]([C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([C:22]#[CH:23])[CH:17]=1)#[CH:15]>>[C:14]([C:16]1[CH:17]=[C:18]([C:22]#[C:23][C:2]2[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][C:10]([O:12][CH3:13])=[O:11])=[CH:4][CH:3]=2)[CH:19]=[CH:20][CH:21]=1)#[CH:15]참가 물질
3
실험 절차
The title compound was prepared from methyl 3-(4-iodophenyl)propanoate (120 mg, 0.41 mmol) and 1,3-diethynylbenzene (0.06 mL, 0.45 mmol) according to the general procedure IC, with the exception that the reaction was performed at room temperature, to give 52 mg (43%) of an yellow-brown gummy oil after purification by flash chromatography (SiO2, EtOAc/hexanes, 1:3). Rf: 0.41 (EtOAc:hexanes, 1:2); 1HNMR (CDCl3) δ 7.65 (s, 1H), 7.49-7.42 (m, 4H), 6.31-7.29 (m, 1H), 7.19-7.17 (m, 2H), 3.67 (s, 3H), 3.09 (s, 1H), 2.99-2.93 (t, 2H, J=7.8 Hz), 2.66-2.61 (t, 2H, J=7.8 Hz); 13CNMR (CDCl3) δ 173.0, 141.1, 135.0, 131.8, 131.7, 128.4, 123.7, 122.4, 120.8, 90.0, 88.0, 82.8, 77.7, 51.6, 35.3, 30.8; EI-MS m/z 288 (M+).
후처리
- customwas performed at room temperature
출처 및 근거
- ORD 기록
- ord-d555a2fea64a4c1fa906fa3e788f8448
- 출처 데이터셋
- uspto-grants-2013_11
- 특허 번호
- US08586607B2
연결된 노트
불러오는 중…