反応式
[CH2:1]([O:15][C:16]1[CH:21]=[CH:20][C:19]([CH2:22][NH2:23])=[CH:18][CH:17]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].[CH:24]1[C:29]2[C:30]([O:32][C:33](=O)[C:28]=2[CH:27]=[N:26][CH:25]=1)=[O:31]>C(Cl)(Cl)Cl>[CH2:1]([O:15][C:16]1[CH:21]=[CH:20][C:19]([CH2:22][N:23]2[C:30](=[O:31])[C:29]3[CH:24]=[CH:25][N:26]=[CH:27][C:28]=3[C:33]2=[O:32])=[CH:18][CH:17]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14]参加物
4
反応条件
- 温度
- 190 °C
実験手順
A mixture of 2.5 g of product from Example 99 and 1.17 g of 3,4-pyridinecarboxylic anhydride is heated, in a sealed tube, at 190° C. for 12 minutes. The cooled crystalline product is dissolved in chloroform, dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The residue is purified by chromatography (silica gel: 30-40% ethyl acetate/hexane) to give 3.12 g of the desired product as colorless crystals.
後処理
- dry with materialdried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe residue is purified by chromatography (silica gel: 30-40% ethyl acetate/hexane)
出典と根拠
- ORDレコード
- ord-3b3f8b7adafa4020a56596e78420f3bf
- 出典データセット
- uspto-grants-1993_05
- 特許番号
- US05208247
関連ノート
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