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Pyridine → HCID 178483597、化合物

HRID 2092437
ノート
印刷プレビュー

反応式

HRID 2092437 の反応式
[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](Cl)=[O:7])=[CH:4][C:3]=1[CH3:11].[CH3:12][O:13][C:14](=[O:20])[CH:15]=[C:16]([NH:18][CH3:19])[CH3:17].N1C=CC=CC=1.Cl.N1C=CC=CC=1>>[CH3:12][O:13][C:14](=[O:20])[CH:15]([C:6](=[O:7])[C:5]1[CH:9]=[CH:10][C:2]([Br:1])=[C:3]([CH3:11])[CH:4]=1)/[C:16](=[N:18]/[CH3:19])/[CH3:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 1049PyridineHCID 2734182Methyl 3-(methylamino)but-2-enoateHCID 70215344-Bromo-3-methylbenzoyl chlorideHCID 10176127Pyridinium chloride

生成物 1

HCID 178483597HCID 178483597、化合物

実験手順

To 4-bromo-3-methyl-benzoyl chloride (40.0 mmoml) in tertahydrofuran (300 mL) wad added 3-methylamino-but-2-enoic acid methyl ester (5.12 g, 40.0 mmol), followed by pyridine (3.2 mL, 40.0 mmol), and the reaction was stirred overnight at room temperature. Solid pyridine hydrochloride coated the flask, so the mixture was decanted, and the solid was washed three times with EtOAc. The combined solutions were concentrated and diluted with EtOAc (500 mL), and the mixture was washed three times with water. The aqueous layer was separated and back-extracted with EtOAc, and the combined organic layers were dried over MgSO4, filtered, and concentrated to give the title compound.

後処理

  1. customso the mixture was decanted
  2. washthe solid was washed three times with EtOAc
  3. concentrationThe combined solutions were concentrated
  4. additiondiluted with EtOAc (500 mL)
  5. washthe mixture was washed three times with water
  6. customThe aqueous layer was separated
  7. extractionback-extracted with EtOAc
  8. dry with materialthe combined organic layers were dried over MgSO4
  9. filtrationfiltered
  10. concentrationconcentrated

出典と根拠

ORDレコード
ord-190c8cd05ba94a16b6d91c8ae021b402
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08440707B2

反応ノート

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