반응식
[CH3:1][CH:2]([OH:5])[CH:3]=[CH2:4].C(N(CC)CC)C.[Cl:13][C:14]1[CH:23]=[C:22]2[C:17]([CH:18]=[CH:19][C:20]([CH2:24][O:25][C:26]3[CH:48]=[CH:47][C:29]4[O:30][CH2:31][C:32]5[CH:45]=[C:44](I)[CH:43]=[CH:42][C:33]=5[CH:34]([O:35][CH:36]5[CH2:41][CH2:40][CH2:39][CH2:38][O:37]5)[C:28]=4[CH:27]=3)=[N:21]2)=[CH:16][C:15]=1[F:49].C(Cl)Cl>C(#N)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[Cl:13][C:14]1[CH:23]=[C:22]2[C:17]([CH:18]=[CH:19][C:20]([CH2:24][O:25][C:26]3[CH:48]=[CH:47][C:29]4[O:30][CH2:31][C:32]5[CH:45]=[C:44]([CH2:4][CH2:3][C:2](=[O:5])[CH3:1])[CH:43]=[CH:42][C:33]=5[CH:34]([O:35][CH:36]5[CH2:41][CH2:40][CH2:39][CH2:38][O:37]5)[C:28]=4[CH:27]=3)=[N:21]2)=[CH:16][C:15]=1[F:49]참가 물질
7
반응물 4
생성물 1
시약·촉매·용매 2
실험 절차
0.2 g of (±)-3-buten-2-ol, 1.4 mg of palladium (II) acetate and 0.27 g of triethylamine were added to 1.36 g of 2-(7-chloro-6-fluoroquinolin-2-yl)methoxy-8-iodo-11-(2-tetrahydropyranyloxy)-6,11-dihydrodibenz[b,e]oxepine obtain in Reference example 73 dissolved in 2.5 ml of acetonitrile and the mixture was refluxed under heating for 5.5 hours. After 60 ml of methylene chloride and 60 ml of ice water were added to this reaction mixture, the organic layer was separated, washed with water and dried over anhydrous sodium sulfate. After the solvent was removed, the residue was applied to silica gel column chromatography to obtain 0.76 g of the title compound.
후처리
- customobtain in Reference example 73
- temperaturethe mixture was refluxed
- temperatureunder heating for 5.5 hours
- customthe organic layer was separated
- washwashed with water
- dry with materialdried over anhydrous sodium sulfate
- customAfter the solvent was removed
출처 및 근거
- ORD 기록
- ord-dea302f230154be58f444459c1e69e67
- 출처 데이터셋
- uspto-grants-1997_01
- 특허 번호
- US05591752
연결된 노트
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