반응식
[CH3:1][C:2]1[S:3][C:4]2[CH:10]=[C:9]([OH:11])[CH:8]=[CH:7][C:5]=2[N:6]=1.[CH2:12]([O:14][C:15](=[O:31])[CH2:16][N:17]1[C:25](=[O:26])[C:24]2[C:19](=[CH:20][CH:21]=[C:22]([N+]([O-])=O)[CH:23]=2)[C:18]1=[O:30])[CH3:13].C(=O)([O-])[O-].[K+].[K+]>CC(N(C)C)=O>[CH2:12]([O:14][C:15](=[O:31])[CH2:16][N:17]1[C:25](=[O:26])[C:24]2[C:19](=[CH:20][CH:21]=[C:22]([O:11][C:9]3[CH:8]=[CH:7][C:5]4[N:6]=[C:2]([CH3:1])[S:3][C:4]=4[CH:10]=3)[CH:23]=2)[C:18]1=[O:30])[CH3:13]참가 물질
5
반응물 3
생성물 1
시약·촉매·용매 1
반응 조건
- 온도
- 105 °C
실험 절차
A mixture of 2-methyl-benzothiazol-6-ol (2.30 g, 13.92 mmol), 5-nitro-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-acetic acid ethyl ester (4.26 g, 15.31 mmol), potassium carbonate (2.3 g, 16.64 mmol) and dimethylacetamide (30 mL) was stirred at 105° C. for twenty hours before it was cooled to room temperature and partitioned between ethyl acetate and water. The organic layer was dried over anhydrous sodium sulfate, concentrated in vacuo and the residue was purified by flash column chromatography on silica gel with a gradient of ethyl acetate and dichloromethane to give the title compound as a yellow solid (2.35 g): MS: (+) m/z 397.19 (M+1).
후처리
- temperaturewas cooled to room temperature
- custompartitioned between ethyl acetate and water
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- concentrationconcentrated in vacuo
- customthe residue was purified by flash column chromatography on silica gel with a gradient of ethyl acetate and dichloromethane
출처 및 근거
- ORD 기록
- ord-3c8457df5c514c929bbe6e2e5e76f01f
- 출처 데이터셋
- uspto-grants-2014_06
- 특허 번호
- US08759373B2
연결된 노트
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