Water → 2-Bromo-5-isocyanato-1,3-dimethylbenzene
反応式
ClC(Cl)(O[C:5](=[O:11])OC(Cl)(Cl)Cl)Cl.[Br:13][C:14]1[C:19]([CH3:20])=[CH:18][C:17]([NH2:21])=[CH:16][C:15]=1[CH3:22].O>O1CCOCC1>[Br:13][C:14]1[C:19]([CH3:20])=[CH:18][C:17]([N:21]=[C:5]=[O:11])=[CH:16][C:15]=1[CH3:22]参加物
5
反応条件
- 温度
- 100 °C
実験手順
Triphosgene (2.23 g, 7.52 mmol) was added to a solution of 4-bromo-3,5-dimethyl-phenylamine (4.3 g, 21.49 mmol) in dioxane (71 ml). After stirring at 100° C. for 15 hours, water was added to the reaction solution. After extraction with ethyl acetate, the organic phase was sequentially washed with water and saturated brine and concentrated under reduced pressure to give 2-bromo-5-isocyanato-1,3-dimethylbenzene (2.0 g, 41%).
後処理
- extractionAfter extraction with ethyl acetate
- washthe organic phase was sequentially washed with water and saturated brine
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-fb602089dde1444fa16869f3eea4d148
- 出典データセット
- uspto-grants-2015_10
- 特許番号
- US09169254B2
反応ノート
読み込み中…