Acetic Acid → Adn 138
반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[O:9][CH2:8][CH2:7][N:6]3[C:10](=[O:24])[C:11]([CH:16](C#N)[C:17](OCC)=[O:18])([C:14]#[N:15])[C:12]([CH:13]=1)=[C:5]23.C(O)(=[O:27])C>S(=O)(=O)(O)O>[Cl:1][C:2]1[CH:3]=[C:4]2[O:9][CH2:8][CH2:7][N:6]3[C:10](=[O:24])[C:11]4([CH2:16][C:17](=[O:18])[NH:15][C:14]4=[O:27])[C:12]([CH:13]=1)=[C:5]23참가 물질
4
실험 절차
A solution of ethyl 2-(8-chloro-6-cyano-2,3-dihydro-5-oxopyrrolo[1,2,3-de]-1,4-benzoxazine-6-yl)-2-cyanoacetate (1 g) in sulfuric acid (0.5 ml)-acetic acid (10 ml) was heated under reflux for 2 hours. The reaction mixture was poured into ice water, and the resulting precipitate was collected by filtration. Recrystallization from acetic acid afforded colorless crystals (0.48 g, 57%), mp 271° C.
후처리
- temperatureunder reflux for 2 hours
- filtrationthe resulting precipitate was collected by filtration
- customRecrystallization from acetic acid afforded colorless crystals (0.48 g, 57%), mp 271° C.
출처 및 근거
- ORD 기록
- ord-7a86ccaeaff94c10b1f804f8c6fdaf39
- 출처 데이터셋
- uspto-grants-1988_08
- 특허 번호
- US04764608
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