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Methyl iodide → 4'-{[5-(4-methoxy-2,2-dimethyl-3,4-dihydro-2H-chromen-6-yl)-4-methyl-6-oxo-2-propylpyrimidin-1(6H)-yl]methyl}biphenyl-2-carbonitrile

HRID 1719075
ノート
印刷プレビュー

反応式

HRID 1719075 の反応式
I[CH3:2].[H-].[Na+].[OH:5][CH:6]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([C:16]3[C:21](=[O:22])[N:20]([CH2:23][C:24]4[CH:29]=[CH:28][C:27]([C:30]5[C:31]([C:36]#[N:37])=[CH:32][CH:33]=[CH:34][CH:35]=5)=[CH:26][CH:25]=4)[C:19]([CH2:38][CH2:39][CH3:40])=[N:18][C:17]=3[CH3:41])[CH:14]=2)[O:9][C:8]([CH3:43])([CH3:42])[CH2:7]1>CN(C)C=O.C(OCC)(=O)C>[CH3:2][O:5][CH:6]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([C:16]3[C:21](=[O:22])[N:20]([CH2:23][C:24]4[CH:29]=[CH:28][C:27]([C:30]5[C:31]([C:36]#[N:37])=[CH:32][CH:33]=[CH:34][CH:35]=5)=[CH:26][CH:25]=4)[C:19]([CH2:38][CH2:39][CH3:40])=[N:18][C:17]=3[CH3:41])[CH:14]=2)[O:9][C:8]([CH3:42])([CH3:43])[CH2:7]1
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 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 594694234'-{[5-(4-hydroxy-2,2-dimethyl-3,4-dihydro-2H-chromen-6-yl)-4-methyl-6-oxo-2-propylpyrimidin-1(6H)-yl]methyl}biphenyl-2-carbonitrile

生成物 1

HCID 594693994'-{[5-(4-methoxy-2,2-dimethyl-3,4-dihydro-2H-chromen-6-yl)-4-methyl-6-oxo-2-propylpyrimidin-1(6H)-yl]methyl}biphenyl-2-carbonitrile収率 66.1%

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of iodomethane (0.76 g), 60% sodium hydride (0.22 g) and 4′-{[5-(4-hydroxy-2,2-dimethyl-3,4-dihydro-2H-chromen-6-yl)-4-methyl-6-oxo-2-propylpyrimidin-1(6H)-yl]methyl}biphenyl-2-carbonitrile (0.56 g) in N,N-dimethylformamide (5 mL) was stirred for 1 hr. The reaction mixture was diluted with ethyl acetate, washed with water, dried over sodium sulfate and concentrated. The residue was purified by silica gel column chromatography to give the title compound as a colorless solid (0.38 g, 66%).

後処理

  1. washwashed with water
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated
  4. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-7bd2e13a980b46b2a3a625e7a8dafe45
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07803940B2

反応ノート

読み込み中…

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