反応式
[Cl-].[Al+3].[Cl-].[Cl-].[C:5](Cl)(=[O:7])[CH3:6].[CH3:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][C:12]=1[CH3:19].Cl>C(Cl)(Cl)(Cl)Cl.C(Cl)Cl>[CH3:18][O:17][C:14]1[CH:13]=[C:12]([CH3:19])[C:11]([O:10][CH3:9])=[CH:16][C:15]=1[C:5](=[O:7])[CH3:6]参加物
実験手順
A suspension of 17.52 g of aluminium chloride in a mixture of 100 ml of CCl4 and 100 ml of DCM is cooled to +4° C. under nitrogen, and 10.4 g of acetyl chloride are added dropwise, followed by a solution of 20 g of 2,5-dimethoxytoluene in 20 ml of DCM. After stirring for 4 hours at +4° C., the reaction medium is poured onto ice to which a few ml of concentrated HCl have been added and the mixture is left stirring for 30 minutes. The phases are separated by settling, the aqueous phase is extracted with DCM and the combined organic phases are washed with aqueous 5% NaCO3 solution, dried over MgSO4 and evaporated. The product crystallizes, and is triturated from 150 ml of heptane, filtered off and then washed with heptane to give 21.03 g of the expected compound: m.p.=75-77° C.
後処理
- temperatureis cooled to +4° C. under nitrogen
- additionhave been added
- waitthe mixture is left
- stirringstirring for 30 minutes
- customThe phases are separated
- extractionthe aqueous phase is extracted with DCM
- washthe combined organic phases are washed with aqueous 5% NaCO3 solution
- dry with materialdried over MgSO4
- customevaporated
- customThe product crystallizes
- customis triturated from 150 ml of heptane
- filtrationfiltered off
- washwashed with heptane
出典と根拠
- ORDレコード
- ord-4dfb60828b9b45c59b2188ac4c1d9331
- 出典データセット
- uspto-grants-2002_04
- 特許番号
- US06380230B1
関連ノート
読み込み中…