반응식
[H-].[Na+].[Li+].[Br-].[Br:5][C:6]1[C:15]([CH2:16]Br)=[CH:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[N:7]=1.[OH2:18].CO[CH2:21][CH2:22][O:23]C.[CH3:25][N:26]([CH:28]=[O:29])C>>[Br:5][C:6]1[C:15]([CH2:16][N:26]2[CH:25]=[CH:13][C:8]3[C:9](=[O:18])[CH2:10][CH:22]([OH:23])[C:21]=3[C:28]2=[O:29])=[CH:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[N:7]=1참가 물질
반응 조건
- 온도
- 80 °C
실험 절차
0.6 mmol (18 mg) of NaH as an 80% dispersion in mineral oil is added in small fractions to a solution, stirred at 0° C. of 0.6 mmol (100 mg) of the compound described in Preparation A in 20 ml of a DME/DMF mixture (16/4 (v/v)). The mixture is stirred at 0° C. for 10 minutes before the addition, at that temperature, of 2.4 mmol (210 mg) of LiBr. After returning to room temperature, the reaction mixture is stirred for ¼ hour before the addition of 0.66 mmol (200 mg) of 2-bromo-3-bromomethylquinoline. The reaction mixture is then heated at 80° C. for 20 hours and, after returning to room temperature, subsequently poured into a large excess of water. The precipitate that forms is filtered off and washed with ether to yield the expected product.
후처리
- customAfter returning to room temperature
- customafter returning to room temperature
- filtrationThe precipitate that forms is filtered off
- washwashed with ether
출처 및 근거
- ORD 기록
- ord-b0f66bd89f8b41cab98c5a373fd8dd35
- 출처 데이터셋
- uspto-grants-2004_03
- 특허 번호
- US06699876B2
연결된 노트
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