Urea → 2-Bromo-4-chlorobenzonitrile
反応式
[Br:1][C:2]1[CH:10]=[C:9]([Cl:11])[CH:8]=[CH:7][C:3]=1[C:4](O)=O.[NH2:12]C(N)=O>ClCCl>[Br:1][C:2]1[CH:10]=[C:9]([Cl:11])[CH:8]=[CH:7][C:3]=1[C:4]#[N:12]参加物
4
実験手順
588 mg of 2-bromo-4-chlorobenzoic acid and 300 mg of urea are dissolved in dichloromethane/methanole and deposited onto 364 mg of aluminum oxide on a rotary evaporator. The residue is irradiated for 60 min in a microwave at 150° C. After cooling the residue is stirred with ethyl acetate and water, the mixture is filtered and the aqueous phase is removed. The organic phase is washed with a sodium hydrogencarbonate solution dried over sodium sulfate, concentrated on a rotary evaporator and then dried under high vacuum. The product is reacted further without additional purification.
後処理
- customdeposited onto 364 mg of aluminum oxide on a rotary evaporator
- customThe residue is irradiated for 60 min in a microwave at 150° C
- temperatureAfter cooling the residue
- filtrationthe mixture is filtered
- customthe aqueous phase is removed
- washThe organic phase is washed with a sodium hydrogencarbonate solution
- dry with materialdried over sodium sulfate
- concentrationconcentrated on a rotary evaporator
- customdried under high vacuum
- customThe product is reacted further without additional purification
出典と根拠
- ORDレコード
- ord-76ae201f062f4fa79013a64f98874d37
- 出典データセット
- uspto-grants-2011_01
- 特許番号
- US07867992B2
反応ノート
読み込み中…