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Cesium carbonate → HCID 86630117、化合物

HRID 1715313
ノート
印刷プレビュー

反応式

HRID 1715313 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

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

生成物 1

HCID 86630117HCID 86630117、化合物

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒
HCID 25517
Ammonium Chloride
溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-ec09882111ee49139e4d4cf6afd797be
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07799820B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート