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Cesium carbonate → HCID 178497098、化合物

HRID 931399
ノート
印刷プレビュー

反応式

HRID 931399 の反応式
Br[C:2]1[C:3]([NH:9][C:10](=[O:25])[C:11](=[CH2:24])[CH:12]([C:14]2[CH:19]=[CH:18][C:17]([C:20]([O:22][CH3:23])=[O:21])=[CH:16][CH:15]=2)[CH3:13])=[N+:4]([O-:8])[CH:5]=[CH:6][CH:7]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C=O)C.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[CH3:23][O:22][C:20]([C:17]1[CH:16]=[C:15]2[C:14](=[CH:19][CH:18]=1)[CH:12]([CH3:13])[C:11]1([C:2]3[C:3](=[N+:4]([O-:8])[CH:5]=[CH:6][CH:7]=3)[NH:9][C:10]1=[O:25])[CH2:24]2)=[O:21]
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

5

反応物 2

HCID 10796Cesium carbonateHCID 178459998HCID 178459998、化合物

生成物 1

HCID 178497098HCID 178497098、化合物

試薬・触媒・溶媒 2

HCID 178418476HCID 178418476、化合物触媒HCID 6228Dimethylformamide溶媒

反応条件

温度
110 °C

実験手順

Bis(triphenylphosphine)palladium(II) dichloride (0.17 g, 0.24 mmol) was added to a deoxygenated mixture of 3-bromo-2-(3-(4-(methoxycarbonyl)phenyl)-2-methylenebutanamido)pyridine 1-oxide (2.0 g, 5.0 mmol), cesium carbonate (4.03 g, 12.4 mmol) in anhydrous DMF (40 mL). The resulting mixture was heated at 110° C. under nitrogen for 20 h, then cooled and filtered through Celite®. The filter cake was washed with ethyl acetate. The filtrate was concentrated, and partitioned between ethyl acetate and brine (2×). The combined organic layers were dried over anhydrous sodium sulfate and concentrated to give the title compound which was used without further purification in next step.

後処理

  1. temperaturecooled
  2. filtrationfiltered through Celite®
  3. washThe filter cake was washed with ethyl acetate
  4. concentrationThe filtrate was concentrated
  5. custompartitioned between ethyl acetate and brine (2×)
  6. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-790f850ee3f84e9fb2f44123c45e04ef
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09296750B2

反応ノート

読み込み中…

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