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Cesium carbonate → 5-[2-(Acetylamino)pyridin-4-yl]-2-(2-chlorophenyl)-3-furoic acid

HRID 537035
ノート
印刷プレビュー

反応式

HRID 537035 の反応式
[C:1]([NH:4][C:5]1[CH:10]=[C:9]([C:11]2[O:15][C:14](Br)=[C:13]([C:17]([O:19]CC)=[O:18])[CH:12]=2)[CH:8]=[CH:7][N:6]=1)(=[O:3])[CH3:2].[Cl:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=1B(O)O.C(=O)([O-])[O-].[Cs+].[Cs+]>O1CCOCC1.O.[OH-].[Na+].C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:1]([NH:4][C:5]1[CH:10]=[C:9]([C:11]2[O:15][C:14]([C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][C:23]=3[Cl:22])=[C:13]([C:17]([OH:19])=[O:18])[CH:12]=2)[CH:8]=[CH:7][N:6]=1)(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 3

HCID 10796Cesium carbonateHCID 27343222-Chlorophenylboronic acidHCID 66748312Ethyl 5-[2-(acetylamino)pyridin-4-yl]-2-bromo-3-furoate

生成物 1

HCID 667483155-[2-(Acetylamino)pyridin-4-yl]-2-(2-chlorophenyl)-3-furoic acid収率 50%

試薬・触媒・溶媒 4

HCID 178418397HCID 178418397、化合物
触媒
HCID 962Water溶媒2 回
HCID 14798Sodium Hydroxide溶媒
HCID 312751,4-Dioxane溶媒

実験手順

To a solution of ethyl 5-[2-(acetylamino)pyridin-4-yl]-2-bromo-3-furoate (0.030 g, 0.09 mmol) in 1,4-dioxane (0.5 mL) and water (0.1 mL) were added tetrakis(triphenylphosphine)palladium(0) (0.010 g, 0.0088 mmol), (2-chlorophenyl)boronic acid (0.018 g, 0.11 mmol), and cesium carbonate (0.087 g, 0.27 mmol). The reaction mixture was subjected to microwave irradiation at 130° C. for 20 min. The reaction mixture was then diluted with water (2 mL) and 1N aqueous sodium hydroxide (0.25 mL) was added. The mixture was allowed to stir at rt overnight. The reaction mixture was extracted with EtOAc and the organic solutions were combined and concentrated. The residue was purified by column chromatography to give 5-[2-(acetylamino)pyridin-4-yl]-2-(2-chlorophenyl)-3-furoic acid (0.015 g, 50%) as a white solid. LCMS (FA): m/z=357.4 (M+H).

後処理

  1. customirradiation at 130° C. for 20 min
  2. additionwas added
  3. extractionThe reaction mixture was extracted with EtOAc
  4. concentrationconcentrated
  5. customThe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-8fa2868fe98d49e692969641acc58991
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08859768B2

反応ノート

読み込み中…

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