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Sodium Carbonate → 3-(2,6-difluoropyridin-4-yl)-1-(phenylsulfonyl)-1H-pyrrolo[2,3-b]pyridine

HRID 68342
ノート
印刷プレビュー

反応式

HRID 68342 の反応式
[C:1]1([S:7]([N:10]2[C:14]3=[N:15][CH:16]=[CH:17][CH:18]=[C:13]3[C:12](B3OC(C)(C)C(C)(C)O3)=[CH:11]2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[F:28][C:29]1[CH:34]=[C:33](I)[CH:32]=[C:31]([F:36])[N:30]=1.C(=O)([O-])[O-].[Na+].[Na+]>C(COC)OC.C(O)C.O.O>[F:28][C:29]1[CH:34]=[C:33]([C:12]2[C:13]3[C:14](=[N:15][CH:16]=[CH:17][CH:18]=3)[N:10]([S:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)(=[O:9])=[O:8])[CH:11]=2)[CH:32]=[C:31]([F:36])[N:30]=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

6

反応物 3

HCID 10340Sodium CarbonateHCID 217473652,6-Difluoro-4-iodopyridineHCID 455881371-(Phenylsulfonyl)-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyrrolo[2,3-b]pyridine

生成物 1

HCID 674403733-(2,6-difluoropyridin-4-yl)-1-(phenylsulfonyl)-1H-pyrrolo[2,3-b]pyridine

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 86587095
Dimethoxyethane ethanol water
溶媒

反応条件

温度
80 °C

実験手順

A suspension of 1-(phenylsulfonyl)-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrrolo[2,3-b]pyridine (7.26 g, 18.9 mmol), 2,6-difluoro-4-iodopyridine (4.14 g, 17.2 mmol, Eur. J. Org. Chem., 2004, 1018 and Org. Lett. 2007, 5175), dichlorobis(triphenylphosphine) palladium(II) (0.482 g, 0.687 mmol) and 1M aqueous sodium carbonate (13.7 mL, 13.7 mmol) in dimethoxyethane/ethanol/water (7:2:3) (80 mL) was degassed and heated at 80° C. for 1.5 hours. After cooling, the suspension was filtered, washed with water and ether, and concentrated to give the crude title compound. The filtrate was diluted with water and extracted twice with dichloromethane. The combined organic layers were dried over magnesium sulfate, filtered, concentrated, and purified using an ISCO Companion flash system eluting with dichloromethane/hexane (7:3 to 9:1) to give the title compound. The combined products were used in the next step without further purification.

後処理

  1. customwas degassed
  2. temperatureAfter cooling
  3. filtrationthe suspension was filtered
  4. washwashed with water and ether
  5. concentrationconcentrated
  6. customto give the crude title compound
  7. extractionextracted twice with dichloromethane
  8. dry with materialThe combined organic layers were dried over magnesium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated
  11. custompurified
  12. washeluting with dichloromethane/hexane (7:3 to 9:1)

出典と根拠

ORDレコード
ord-80918da8537a479b9642295842d347d7
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822446B2

反応ノート

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