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Dimethylformamide → HCID 22227893、化合物

HRID 1744563
ノート
印刷プレビュー

反応式

HRID 1744563 の反応式
[CH3:1]N(C)C=O.[C:6]([C:8]1[CH:9]=[C:10]([NH:20][C:21]([C:23]2[C:24]([CH3:35])=[N:25][N:26]([C:28]3[CH:33]=[CH:32][C:31]([F:34])=[CH:30][CH:29]=3)[CH:27]=2)=[O:22])[CH:11]=[CH:12][C:13]=1[O:14][CH2:15][C:16]([CH3:19])([CH3:18])[CH3:17])#[N:7].[H-].[Na+].CI>O>[C:6]([C:8]1[CH:9]=[C:10]([N:20]([CH3:1])[C:21]([C:23]2[C:24]([CH3:35])=[N:25][N:26]([C:28]3[CH:33]=[CH:32][C:31]([F:34])=[CH:30][CH:29]=3)[CH:27]=2)=[O:22])[CH:11]=[CH:12][C:13]=1[O:14][CH2:15][C:16]([CH3:19])([CH3:18])[CH3:17])#[N:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228Dimethylformamide2 回HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 9909290N-(3-Cyano-4-neopentyloxyphenyl)-1-(4-fluorophenyl)-3-methylpyrazole-4-carboxamide

生成物 1

HCID 22227893HCID 22227893、化合物

試薬・触媒・溶媒 1

HCID 962Water
溶媒

実験手順

To dimethylformamide (5 ml) solution containing N-(3-cyano-4-neopentyloxyphenyl)-1-(4-fluorophenyl)-3-methylpyrazole-4-carboxamide (1.5 g) was added sodium hydride (60% content, 0.2 g) under ice-cooling and the mixture was stirred for 1 h. A solution of dimethylformamide (1 ml) containing methyl iodide (0.6 g) was added and the mixture was stirred under ice-cooling for 1 h. The mixture was allowed to warm to room temperature and stirred for 1 h. The reaction mixture was added into water and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate, after which the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (mobile phase: ethyl acetate:n-hexane=5:1) to give the title compound (0.5 g), melting point: 65–69° C.

後処理

  1. temperaturecooling
  2. additionwas added
  3. stirringthe mixture was stirred under ice-
  4. temperaturecooling for 1 h
  5. stirringstirred for 1 h
  6. extractionextracted with ethyl acetate
  7. washThe organic layer was washed with saturated brine
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customafter which the solvent was evaporated under reduced pressure
  10. customThe residue was purified by silica gel column chromatography (mobile phase: ethyl acetate:n-hexane=5:1)

出典と根拠

ORDレコード
ord-20e4e001f5b2496b886f8e450f9dd4be
出典データセット
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07015218B1

反応ノート

読み込み中…

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