Water → 3-Ethynylpyridine-2,6-diamine
反応式
C[Si]([C:5]#[C:6][C:7]1[C:8]([NH2:14])=[N:9][C:10]([NH2:13])=[CH:11][CH:12]=1)(C)C.[F-].C([N+](CCCC)(CCCC)CCCC)CCC.O>O1CCCC1>[C:6]([C:7]1[C:8]([NH2:14])=[N:9][C:10]([NH2:13])=[CH:11][CH:12]=1)#[CH:5]参加物
5
実験手順
To a solution of 3-trimethylsilanylethynyl-pyridin-2,6-diamine (7.0 g, 34.1 mmoL) described in Manufacturing Example 13-1-2 in tetrahydrofuran (100 mL) was added tetrabutylammonium fluoride (1M tetrahydrofuran solution, 17 mL, 17 mmol) on an ice bath, which was stirred for 10 minutes at room temperature. Water was added to the reaction solution, which was then extracted with ethyl acetate 3 times. The extract was dried over sodium sulfate, and the solvent was evaporated under a reduced pressure. The residue was purified by silica gel chromatography (ethyl acetate) to obtain the title compound (3.35 g, 73.8%).
後処理
- extractionwas then extracted with ethyl acetate 3 times
- dry with materialThe extract was dried over sodium sulfate
- customthe solvent was evaporated under a reduced pressure
- customThe residue was purified by silica gel chromatography (ethyl acetate)
出典と根拠
- ORDレコード
- ord-9bfab83f2eb7466e9bc8c3324ee34706
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08841327B2
反応ノート
読み込み中…