Hydrochloric Acid → 2-(2-hydroxymethylphenyl)-2-methoxyimino-N-methylacetamide

HRID 1857818ノート

反応式

HRID 1857818 の反応式
CO.Cl.[CH3:4][O:5][N:6]=[C:7]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[CH2:18][O:19]C1CCCCO1)[C:8]([NH:10][CH3:11])=[O:9]>[Cl-].[Na+].O>[OH:19][CH2:18][C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=1[C:7](=[N:6][O:5][CH3:4])[C:8]([NH:10][CH3:11])=[O:9]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 53869643HCID 53869643、化合物

生成物 1

HCID 544725602-(2-hydroxymethylphenyl)-2-methoxyimino-N-methylacetamide収率 94.6%

試薬・触媒・溶媒 1

HCID 57417360Sodium chloride; water溶媒

実験手順

Methanol (2 ml) and a 36% aqueous hydrochloric acid solution (0.01 g, 0.0001 mol) were added to an E/Z mixture of 2-methoxyimino-N-methyl-2-[2-(2-tetrahydropyranyloxymethyl)phenyl]acetamide (0.31 g, 0.001 mol), and the mixture was stirred at room temperature for 30 minutes. After completion of the reaction, half-saturated brine (80 ml) was added, and the mixture was extracted with dichloromethane (50 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 2-(2-hydroxymethylphenyl)-2-methoxyimino-N-methylacetamide (0.21 g, Yield: 94.6%, E/Z=97/3) as colorless crystals.

後処理

  1. additionwas added
  2. extractionthe mixture was extracted with dichloromethane (50 ml) twice
  3. dry with materialThe extract was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting residue was purified by silica gel chromatography (ethyl acetate/n-hexane)

出典と根拠

ORDレコード
ord-c185cc7c436440ff96d1c8d3080623bf
出典データセット
uspto-grants-2000_11
特許番号
US06147231

反応ノート

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