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Ethyl orthoformate → HCID 136337142、化合物

HRID 519659
ノート
印刷プレビュー

反応式

HRID 519659 の反応式
[CH2:1]([C:5]1[N:6]=[C:7]([NH:27][NH2:28])[NH:8][C:9](=[O:26])[C:10]=1[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([C:18]2[C:19]([C:24]#[N:25])=[CH:20][CH:21]=[CH:22][CH:23]=2)=[CH:14][CH:13]=1)[CH2:2][CH2:3][CH3:4].[CH:29](OCC)(OCC)OCC>>[CH2:1]([C:5]1[N:6]2[CH:29]=[N:28][N:27]=[C:7]2[NH:8][C:9](=[O:26])[C:10]=1[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([C:18]2[C:19]([C:24]#[N:25])=[CH:20][CH:21]=[CH:22][CH:23]=2)=[CH:14][CH:13]=1)[CH2:2][CH2:3][CH3:4]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 31214Ethyl orthoformateHCID 136337141HCID 136337141、化合物

生成物 1

HCID 136337142HCID 136337142、化合物収率 17%

反応条件

温度
100 °C

実験手順

A mixture of 4′-[(4-butyl-2-hydrazino-6-oxo-1,6-dihydropyrimidin-5-yl)methyl]biphenyl-2-carbonitrile (2.6 g) and triethyl orthoformate (30 mL) was stirred at 100° C. for 16 hr. The reaction mixture was concentrated, and ethyl acetate and water were added to the obtained residue. The ethyl acetate layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to give the title compound as a colorless solid (0.46 g, 17%).

後処理

concentration
The reaction mixture was concentrated
  • additionethyl acetate and water were added to the obtained residue
  • washThe ethyl acetate layer was washed with saturated brine
  • dry with materialdried over anhydrous magnesium sulfate
  • customThe solvent was evaporated under reduced pressure
  • customThe obtained residue was purified by silica gel column chromatography
  • 出典と根拠

    ORDレコード
    ord-483fd2a0b5b74ff8ac34226d35cd90f7
    出典データセット
    uspto-grants-2015_08
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US09115136B2

    反応ノート

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    このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート