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Cesium carbonate → HCID 86630117, 화합물

HRID 1715313
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HRID 1715313 반응식
C(=O)([O-])[O-].[Cs+].[Cs+].CN1CCCC1=O.[Cl:14][C:15]1[C:20]([OH:21])=[CH:19][CH:18]=[CH:17][N:16]=1.Cl[C:23]1[CH:24]=[CH:25][C:26]([S:29]([CH2:32][CH3:33])(=[O:31])=[O:30])=[N:27][CH:28]=1>C(OCC)(=O)C.[Cl-].[NH4+]>[Cl:14][C:15]1[C:20]([O:21][C:23]2[CH:28]=[N:27][C:26]([S:29]([CH2:32][CH3:33])(=[O:30])=[O:31])=[CH:25][CH:24]=2)=[CH:19][CH:18]=[CH:17][N:16]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 10796Cesium carbonateHCID 13387N-methyl-2-pyrrolidoneHCID 811362-Chloro-3-pyridinolHCID 231451535-Chloro-2-(ethanesulfonyl)pyridine

생성물 1

HCID 86630117HCID 86630117, 화합물

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매
HCID 25517
Ammonium Chloride
용매

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온도
100 °C

실험 절차

Cesium carbonate (20 g) was added to an N-methyl-2-pyrrolidinone (160 ml) solution of 2-chloro-3-hydroxypyridine (6 g) and 5-chloro-2-(ethylsulfonyl)pyridine (4.8 g), and stirred at 100° C. for 24 hours. After this was diluted with ethyl acetate, aqueous saturated ammonium chloride solution was added with cooling with ice. The organic layer was washed with water and saturated saline water. After dried, the solvent was evaporated away under reduced pressure, and the residue was purified by silica gel column chromatography (developing solvent: hexane/ethyl acetate) to obtain the entitled compound as a brown oil.

후처리

  1. additionwas added
  2. temperaturewith cooling with ice
  3. washThe organic layer was washed with water and saturated saline water
  4. customAfter dried
  5. customthe solvent was evaporated away under reduced pressure
  6. customthe residue was purified by silica gel column chromatography (developing solvent: hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-ec09882111ee49139e4d4cf6afd797be
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07799820B2

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