Water → 3-[5-[2-(4-Dibutylamino-2-methoxyphenyl)vinyl]thiophene-2-yl]acrylonitrile
反応式
[H-].[Na+].[C:3]([CH2:5]P(=O)(OCC)OCC)#[N:4].[CH2:14]([N:18]([CH2:36][CH2:37][CH2:38][CH3:39])[C:19]1[CH:24]=[CH:23][C:22]([CH:25]=[CH:26][C:27]2[S:31][C:30]([CH:32]=O)=[CH:29][CH:28]=2)=[C:21]([O:34][CH3:35])[CH:20]=1)[CH2:15][CH2:16][CH3:17].O>O1CCCC1>[CH2:14]([N:18]([CH2:36][CH2:37][CH2:38][CH3:39])[C:19]1[CH:24]=[CH:23][C:22]([CH:25]=[CH:26][C:27]2[S:31][C:30]([CH:32]=[CH:5][C:3]#[N:4])=[CH:29][CH:28]=2)=[C:21]([O:34][CH3:35])[CH:20]=1)[CH2:15][CH2:16][CH3:17]参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
To 111 mg (4.63 mmol) of sodium hydride, 8 ml of tetrahydrofuran was added. To this mixture, 820 mg (4.63 mmol) of diethyl cyanomethylphosphonate was added dropwise under ice cooling, and the mixture was stirred for 30 minutes. Next, 860 mg (2.31 mmol) of 5-[2-(4-dibutylamino-2-methoxyphenyl)vinyl]thiophene-2-carboaldehyde in tetrahydrofuran was added dropwise, and the mixture was stirred for 1 hour. The reaction mixture was poured into water and subjected to extraction with ethyl acetate. The extract was washed with a saturated saline solution, dried over anhydrous sodium sulfate, and concentrated. The residue was purified by silica gel column chromatography to give 828 mg of a deep red oily matter (yield: 90.7%).
後処理
- stirringthe mixture was stirred for 1 hour
- extractionsubjected to extraction with ethyl acetate
- washThe extract was washed with a saturated saline solution
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated
- customThe residue was purified by silica gel column chromatography
- customto give 828 mg of a deep red oily matter (yield: 90.7%)
出典と根拠
- ORDレコード
- ord-f71b300b87df400391f69adfa468627c
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846955B2
反応ノート
読み込み中…