N,N-Dimethylaniline → HCID 14068732、化合物
反応式
C([O:4][C:5]1[CH:12]=[C:11]([O:13][CH3:14])[CH:10]=[CH:9][C:6]=1[CH:7]=[O:8])C=C.CN(C)[C:17]1[CH:22]=CC=C[CH:18]=1>>[CH2:22]([C:12]1[C:5]([OH:4])=[C:6]([CH:9]=[CH:10][C:11]=1[O:13][CH3:14])[CH:7]=[O:8])[CH:17]=[CH2:18]参加物
3
実験手順
Heat a solution of 125 g of the product obtained in Step A in 300 ml of N,N-dimethylaniline at 200° C. for 15 hours. Then evaporate off the solvent in vacuo and take up the residue in 1 liter of isopropyl ether; extract the solution 10 times using 100 ml of 1N sodium hydroxide solution each time and then acidify the combined extracts using 3N hydrochloric acid. Then extract the aqueous acid solution with dichloromethane, and dry and concentrate the organic phase.
後処理
- customThen evaporate off the solvent in vacuo
- extractionextract the solution 10 times
- extractionThen extract the aqueous acid solution with dichloromethane
- customdry
- concentrationconcentrate the organic phase
出典と根拠
- ORDレコード
- ord-63ae5f1428f142c4be6377684e229960
- 出典データセット
- uspto-grants-2004_06
- 特許番号
- US06747032B2
反応ノート
読み込み中…