Dimethylformamide → HCID 13393792、化合物
反応式
[CH3:1][O:2][C:3]1[C:12]([O:13][CH3:14])=[C:11]([O:15][CH3:16])[CH:10]=[C:9]2[C:4]=1[C:5](=O)[CH2:6][CH:7]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[O:8]2.P(Cl)(Cl)([Cl:26])=O.CN(C)[CH:31]=[O:32]>>[Cl:26][C:5]1[C:4]2[C:9](=[CH:10][C:11]([O:15][CH3:16])=[C:12]([O:13][CH3:14])[C:3]=2[O:2][CH3:1])[O:8][CH:7]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:6]=1[CH:31]=[O:32]参加物
4
実験手順
As in example 1, but using 15 g 5,6,7-trimethoxyflavanone, 150 ml dimethylformamide and 26 ml phosphorous oxychloride. Reaction time is forty eight hours at room temperature. After hydrolysis and usual work up, the residual solid is purified by preparative HPLC and the best fractions are crystallised in hexane. 4-chloro-3-formyl-5,6,7-trimethoxyflav-3-ene is obtained as yellow crystals; m.p. 84°-87° C.
後処理
- customReaction time