反応式
[CH3:1][C:2]1([CH3:17])[CH2:11][CH2:10][C:9]([CH3:13])([CH3:12])[C:8]2[CH:7]=[C:6]([C:14](Cl)=[O:15])[CH:5]=[CH:4][C:3]1=2.C[Si]([C:22]#[C:23][C:24]1[CH:33]=[CH:32][C:27]([C:28]([O:30][CH3:31])=[O:29])=[CH:26][CH:25]=1)(C)C.[Al+3].[Cl-].[Cl-].[Cl-]>ClCCl>[O:15]=[C:14]([C:6]1[CH:5]=[CH:4][C:3]2[C:2]([CH3:17])([CH3:1])[CH2:11][CH2:10][C:9]([CH3:13])([CH3:12])[C:8]=2[CH:7]=1)[C:22]#[C:23][C:24]1[CH:33]=[CH:32][C:27]([C:28]([O:30][CH3:31])=[O:29])=[CH:26][CH:25]=1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
8.4 g (36 mmol) of 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthoyl chloride, 6.9 g (29.7 mmol) of methyl 4-trimethylsilylethynylbenzoate and 100 ml of dichloromethane are introduced into a round-bottomed flask. 16.8 g (125 mmol) of AlCl3 are added portionwise at 0° C. and the mixture is stirred at room temperature for 8 hours. The reaction medium is poured into ice and extracted with dichloromethane, and the organic phase is separated out after settling has taken place, dried over magnesium sulphate and evaporated. The residue obtained is purified by chromatography on a column of silica eluted with a mixture of dichloromethane and hexane (50/50% by volume). 6.8 g (61%) of the expected product are collected, with a melting point of 113-4° C.
後処理
- additionThe reaction medium is poured into ice
- extractionextracted with dichloromethane
- customthe organic phase is separated out after settling
- dry with materialdried over magnesium sulphate
- customevaporated
- customThe residue obtained
- customis purified by chromatography on a column of silica
- washeluted with a mixture of dichloromethane and hexane (50/50% by volume)
- custom6.8 g (61%) of the expected product are collected, with a melting point of 113-4° C.
出典と根拠
- ORDレコード
- ord-e01264b5fb444276bc0a7c64dfa92a4d
- 出典データセット
- uspto-grants-2001_11
- 特許番号
- US06313162B1
関連ノート
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