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

HRID 342183ノート

反応式

HRID 342183 の反応式
CO.[OH:3][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11](=[N:16][O:17][CH3:18])[C:12]([NH:14][CH3:15])=[O:13].Cl.CON=C(C1C=CC=CC=1COC1CCCCO1)C(NC)=O>[Cl-].[Na+].O>[OH:3][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11](=[N:16][O:17][CH3:18])[C:12]([NH:14][CH3:15])=[O:13]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 53869643HCID 53869643、化合物HCID 867535212-(2-hydroxymethylphenyl)-2-methoxyimino-N-methylacetamide Methanol

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

Preparation of 2-(2-hydroxymethylphenyl)-2-methoxyimino-N-methylacetamide 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-d815929c9aa1476199258f8bb96ef56a
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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