Hydrochloric Acid → (2E)-2-[2-[[5-chloro-3-(trifluoromethyl)-2-pyridinyl]oxymethyl]phenyl]-2-methoxyimino-N-methylacetamide

HRID 342187ノート

反応式

HRID 342187 の反応式
[OH:1][CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9](=[N:14][O:15][CH3:16])[C:10]([NH:12][CH3:13])=[O:11].[H-].[Na+].Cl[C:20]1[C:25]([C:26]([F:29])([F:28])[F:27])=[CH:24][C:23]([Cl:30])=[CH:22][N:21]=1.Cl>C1COCC1>[Cl:30][C:23]1[CH:24]=[C:25]([C:26]([F:29])([F:27])[F:28])[C:20]([O:1][CH2:2][C:3]2[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=2/[C:9](=[N:14]\[O:15][CH3:16])/[C:10]([NH:12][CH3:13])=[O:11])=[N:21][CH:22]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 110421442,5-dichloro-3-(trifluoromethyl)pyridineHCID 544725602-(2-hydroxymethylphenyl)-2-methoxyimino-N-methylacetamide

生成物 1

HCID 22016901(2E)-2-[2-[[5-chloro-3-(trifluoromethyl)-2-pyridinyl]oxymethyl]phenyl]-2-methoxyimino-N-methylacetamide収率 74%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

2-(2-Hydroxymethylphenyl)-2-methoxyimino-N-methylacetamide (300 mg) was dissolved in THF (5 ml). 40% sodium hydride (65 mg) was added, and the mixture was stirred for 10 minutes. 2,5-Dichloro-3-trifluoromethylpyridine (350 mg) was added, and the mixture was stirred at room temperature for 12 hours. The mixture was neutralized with 1N-hydrochloric acid and extracted with ethyl acetate. The resulting organic layer was dried over MgSO4, and the solvent was evaporated under reduced pressure. The resulting residue was purified by column chromatography on silica gel to obtain the title compound (398 mg, Yield: 74%).

後処理

  1. stirringthe mixture was stirred at room temperature for 12 hours
  2. extractionextracted with ethyl acetate
  3. dry with materialThe resulting organic layer was dried over MgSO4
  4. customthe solvent was evaporated under reduced pressure
  5. customThe resulting residue was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-fca8ef0de2ad4c0587a2a7a818a94e8a
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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