Diethyl Ether → Chloroisovaniline
反応式
[O:1]=[CH:2][C:3]1[CH:11]=[CH:10][C:7]([O:8][CH3:9])=[C:5]([OH:6])[CH:4]=1.C(O[Cl:17])(C)(C)C.CCOCC>CC(O)=O>[Cl:17][C:4]1[C:5]([OH:6])=[C:7]([O:8][CH3:9])[CH:10]=[CH:11][C:3]=1[CH:2]=[O:1]参加物
5
実験手順
41.2 g (0.271 mol) of isovanillin was dissolved in 160 ml of 90% AcOH under heating. 29.41 g of t-BuOCl was added dropwise to the solution while it was kept at 35° to 40° C. The solution was stirred at room temperature for 3 hours and then 200 ml of ether was added thereto. The mixture was left to stand overnight and crystals thus formed were separated by filtration and washed with ether. 42.0 g of the crude crystals were recrystallized from acetonitrile to obtain 35 g of 2-chloro-3-hydroxy-4-methoxybenzaldehyde (69%).
後処理
- temperatureunder heating
- customwas kept at 35° to 40° C
- waitThe mixture was left
- waitto stand overnight
- customcrystals thus formed
- customwere separated by filtration
- washwashed with ether
- custom42.0 g of the crude crystals were recrystallized from acetonitrile
出典と根拠
- ORDレコード
- ord-340794740b714766947331040402f084
- 出典データセット
- uspto-grants-1994_03
- 特許番号
- US05292521
反応ノート
読み込み中…