Water → HCID 73446014、化合物
反応式
[N-:1]=[N+:2]=[N-:3].[Na+].O.[C:6]([C:8]([C:13]1[S:14][CH:15]=[CH:16][CH:17]=1)=[CH:9][C:10](Cl)=[O:11])#[N:7]>O1CCOCC1>[C:6]([C:8]([C:13]1[S:14][CH:15]=[CH:16][CH:17]=1)=[CH:9][C:10]([N:1]=[N+:2]=[N-:3])=[O:11])#[N:7]参加物
5
実験手順
To a vigorously stirring suspension of NaN3 (55 g, 0.85 mol) in 1:1; dioxane:H2O (200 mL) cooled to 0° C. was added dropwise over 20 min a solution of 3-cyano-3-thiophen-2-yl-acryloyl chloride 22 (84.3 g, 0.428 mol) in dioxane (150 mL). After stirring at 0° C. for 20 min, the reaction was warmed to room temperature and stirred for 1 h. To the reaction solution was added 600 mL H2O, thus producing a precipitate which was filtered, washed with H2O and dried under vacuum to provide pure 85 g of 23.
後処理
- stirringAfter stirring at 0° C. for 20 min
- stirringstirred for 1 h
- customthus producing a precipitate which
- filtrationwas filtered
- washwashed with H2O
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-0a4ef43ad62e469b8a23c595fcfd7835
- 出典データセット
- uspto-grants-2009_12
- 特許番号
- US07635695B2
反応ノート
読み込み中…