反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][NH:8][C:9](=[O:31])[C:10]1[CH:15]=[CH:14][C:13]([O:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])=[CH:12][CH:11]=1.[CH2:32]([I:34])[CH3:33]>>[I-:34].[CH2:32]([N+:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][NH:8][C:9](=[O:31])[C:10]1[CH:11]=[CH:12][C:13]([O:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])=[CH:14][CH:15]=1)[CH3:33]参加物
3
反応条件
- 温度
- 140 °C
実験手順
A mixture of 1.0 g of product from Example 4 and 9.42 ml of ethyl iodide is heated, in a sealed dark tube, at 140° C. for 20 hours. The cooled reaction mixture is concentrated in vacuo, the residue purified by column chromatography (silica gel:10% methyl alcohol/chloroform) and recrystallized from 5% chloroform/methyl alcohol to give 0.96 g of the desired product.
後処理
- customThe cooled reaction mixture
- concentrationis concentrated in vacuo
- customthe residue purified by column chromatography (silica gel:10% methyl alcohol/chloroform)
- customrecrystallized from 5% chloroform/methyl alcohol
出典と根拠
- ORDレコード
- ord-58e62dd22d0241b4a70948708cab22d3
- 出典データセット
- uspto-grants-1993_05
- 特許番号
- US05208247
関連ノート
読み込み中…