Pyridine → HCID 53869643、化合物

HRID 342181ノート

反応式

HRID 342181 の反応式
Cl.[CH3:2][O:3][NH2:4].N1C=CC=CC=1.[CH3:11][NH:12][C:13](=[O:30])[C:14](=O)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[CH2:21][O:22][CH:23]1[CH2:28][CH2:27][CH2:26][CH2:25][O:24]1>CO.[Cl-].[Na+].O>[CH3:2][O:3][N:4]=[C:14]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[CH2:21][O:22][CH:23]1[CH2:28][CH2:27][CH2:26][CH2:25][O:24]1)[C:13]([NH:12][CH3:11])=[O:30]

参加物

6

反応物 3

HCID 1049PyridineHCID 521874O-Methylhydroxylamine hydrochlorideHCID 18357814HCID 18357814、化合物

生成物 1

HCID 53869643HCID 53869643、化合物収率 60.4%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 57417360Sodium chloride; water溶媒

実験手順

Methoxyamine hydrochloride (0.33 g, 0.004 mol) was dissolved in methanol (4 ml), and pyridine (0.47 g, 0.006 mol) was added to the solution. To the mixture was added a mixed solution of N-methyl-2-oxo-2-[2-(2-tetrahydropyranyloxymethyl)phenyl]acetamide (0.55 g, 0.002 mol) and methanol (2 ml). The mixture was stirred under reflux for 2 hours. After completion of the reaction, half-saturated brine (100 ml) was added, and the mixture was extracted with dichloromethane (80 ml) twice. The extract was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (ethyl acetate/n-hexane) to obtain an E/Z mixture of 2-methoxyimino-N-methyl-2-[2-(2-tetrahydropyranyloxymethyl)phenyl]acetamide (0.37 g, Yield: 60.4%) as a colorless oil.

後処理

  1. temperatureunder reflux for 2 hours
  2. additionwas added
  3. extractionthe mixture was extracted with dichloromethane (80 ml) twice
  4. dry with materialThe extract was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting residue was purified by silica gel chromatography (ethyl acetate/n-hexane)
  7. customto obtain

出典と根拠

ORDレコード
ord-e6093a031e864708919aada10d14c2ab
出典データセット
uspto-grants-1999_01
特許番号
US05856573

反応ノート

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