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Cesium carbonate → HCID 86712402, 화합물

HRID 2174197
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HRID 2174197 반응식
Br[C:2]1[C:3]([C:8]([CH3:12])([CH3:11])[CH:9]=[O:10])=[N:4][CH:5]=[CH:6][CH:7]=1.[F:13][C:14]1[CH:15]=[CH:16][CH:17]=[C:18]2[C:23]=1[N:22]=[CH:21][C:20]([OH:24])=[CH:19]2.C(=O)([O-])[O-].[Cs+].[Cs+].C(CC(=O)C(C)(C)C)(=O)C(C)(C)C>CN1CCCC1=O.[Cu]Cl>[F:13][C:14]1[CH:15]=[CH:16][CH:17]=[C:18]2[C:23]=1[N:22]=[CH:21][C:20]([O:24][C:2]1[C:3]([C:8]([CH3:12])([CH3:11])[CH:9]=[O:10])=[N:4][CH:5]=[CH:6][CH:7]=1)=[CH:19]2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 10796Cesium carbonateHCID 707002,2,6,6-Tetramethyl-3,5-heptanedioneHCID 682880678-fluoroquinolin-3-olHCID 86712401HCID 86712401, 화합물

생성물 1

HCID 86712402HCID 86712402, 화합물수율 34.1%

시약·촉매·용매 2

HCID 62652Cuprous chloride
촉매
HCID 13387N-methyl-2-pyrrolidone용매

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온도
130 °C

실험 절차

0.41 g of 2-(3-bromo-pyridin-2-yl)-2-methyl-propioaldehyde were dissolved in 4 ml of N-methylpyrrolidone. 0.59 g of 8-fluoro-3-hydroxyquinoline, 1.2 g of cesium carbonate, 0.07 g of dipivaloylmethane and 0.18 g of copper (I) chloride were added thereto followed by stirring for 16 hours at 130° C. Subsequently, the reaction solution was cooled to room temperature and purified by silica gel column chromatography to obtain 0.19 g of 2-[3-(8-fluoro-quinolin-3-yloxy)-pyridin-2-yl]-2-methyl-propioaldehyde.

후처리

  1. temperatureSubsequently, the reaction solution was cooled to room temperature
  2. custompurified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-eadc2c79f80849ab90c59f73ca1314f0
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09060517B2

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