反応式
Cl[C:2]([O:4][CH2:5][CH3:6])=[O:3].OC1C=[C:24]([O:26][CH3:27])[CH:23]=[C:22]([O:28][CH3:29])[C:9]=1[C:10](=[O:21])[CH:11]=[CH:12][C:13]1[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][CH:14]=1.[OH2:30].N1[CH:36]=[CH:35]C=CC=1>>[CH2:35]([O:3][C:2]([O:4][C:5]1[CH:6]=[C:24]([O:26][CH3:27])[CH:23]=[C:22]([O:28][CH3:29])[C:9]=1[C:10](=[O:21])[CH:11]=[CH:12][C:13]1[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][CH:14]=1)=[O:30])[CH3:36]参加物
5
実験手順
Ethyl chloroformate (216 mg) was added dropwise to a solution of 2'-hydroxy-4,4',6'-trimethoxychalcone (314 mg) in 5 ml of pyridine. After stirring at room temperature for 30 minutes, the mixture was poured into water (30 ml). The mixture was extracted with three 30 ml portions of chloroform, and the combined extracts were washed with water, dried over Na2SO4 and evaporated to give an oily residue. Crystallization of the residue from methanol gave 202 mg (53% yield) of 2'-(ethoxycarbonyloxy)4,4',6'-trimethoxychalcone as pale yellow prisms; m.p. 107° C.
後処理
- extractionThe mixture was extracted with three 30 ml portions of chloroform
- washthe combined extracts were washed with water
- dry with materialdried over Na2SO4
- customevaporated
- customto give an oily residue
- customCrystallization of the residue from methanol
出典と根拠
- ORDレコード
- ord-886c005a8ab34ef0b612cdf910c5845e
- 出典データセット
- uspto-grants-1986_08
- 特許番号
- US04605674
関連ノート
読み込み中…