反応式
[C:1]([O:7][CH2:8][N:9]=[N+:10]=[N-:11])(=[O:6])[C:2]([CH3:5])([CH3:4])[CH3:3].O.C(O)CCC.[CH2:18]([O:21][C:22]1[CH:23]=[CH:24][C:25]([N:28]2[CH:32]=[N:31][N:30]=[N:29]2)=[N:26][CH:27]=1)[C:19]#[CH:20].O=C1O[C@H]([C@H](CO)O)C([O-])=C1O.[Na+]>O.S([O-])([O-])(=O)=O.[Cu+2]>[C:1]([O:7][CH2:8][N:9]1[CH:20]=[C:19]([CH2:18][O:21][C:22]2[CH:27]=[N:26][C:25]([N:28]3[CH:32]=[N:31][N:30]=[N:29]3)=[CH:24][CH:23]=2)[N:11]=[N:10]1)(=[O:6])[C:2]([CH3:5])([CH3:4])[CH3:3]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
To a solution of azidomethyl pivalate (4.26 g, 27.1 mmol) in 1:1 text -butanol water (90 mL total) was added 5-(prop-2-ynyloxy)-2-(1H-tetrazol-1-yl)pyridine (5.45 g, 27.1 mmol), sodium ascorbate (1.4 mL of a 1M solution in water) and copper sulfate (1.4 mL of a 1M solution in water). The solution was stirred at room temperature for 72 hours. Water was added and the suspension was extracted with ethyl acetate. The organic layer was separated, dried over sodium sulfate, filtered and concentrated in vacuo to afford the expected product which was used in the next step without further purification. 1H NMR (DMSO-d6): δ 10.07 (1H, s), 8.43-8.41 (2H, m), 8.00 (1H, d, J=8.8 Hz), 7.88 (1H, dd, J=3.2, 8.8 Hz), 6.32 (2H, s), 5.38 (2H, s), 1.08 (9H, s).
後処理
- extractionthe suspension was extracted with ethyl acetate
- customThe organic layer was separated
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-6cb9a023f229469fa1e8821c6da6f32f
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846675B2
関連ノート
読み込み中…