反応式
Br[C:2]1[CH:3]=[C:4](/[C:7](/[CH2:24][CH3:25])=[CH:8]/[CH2:9][CH2:10][C:11]([CH2:22][CH3:23])([CH2:20][CH3:21])[O:12][Si:13]([CH2:18][CH3:19])([CH2:16][CH3:17])[CH2:14][CH3:15])[S:5][CH:6]=1.C([Li])CCC.CN(C)[CH:33]=[O:34].[Cl-].[NH4+]>C1COCC1>[CH2:24](/[C:7](/[C:4]1[S:5][CH:6]=[C:2]([CH:33]=[O:34])[CH:3]=1)=[CH:8]\[CH2:9][CH2:10][C:11]([CH2:22][CH3:23])([O:12][Si:13]([CH2:18][CH3:19])([CH2:16][CH3:17])[CH2:14][CH3:15])[CH2:20][CH3:21])[CH3:25]参加物
6
反応条件
- 温度
- -78 °C
実験手順
11 g (24.7 mmol) of [(E)-5-(4-bromo-2-thienyl)-1,1-diethylhept-4-enyloxy]triethylsilane are dissolved in 100 mL of anhydrous THF and the mixture is cooled to −78° C. 10.9 mL (27 mmol) of 2.5 M butyllithium are added slowly and the mixture is stirred for 15 minutes. 2.1 mL (27 mmol) of dimethylformamide are then added and the medium is stirred for 30 minutes and then poured into aqueous ammonium chloride solution. After extraction with ethyl acetate and chromatography on silica gel (eluent: 9 heptane/1 ethyl acetate), the product is obtained in the form of a colourless oil (m=4 g; Y=41%).
後処理
- stirringthe medium is stirred for 30 minutes
- extractionAfter extraction with ethyl acetate and chromatography on silica gel (eluent: 9 heptane/1 ethyl acetate)
- customthe product is obtained in the form of a colourless oil (m=4 g; Y=41%)
出典と根拠
- ORDレコード
- ord-6dbcfd73dfe4425bbfccfb8343299adb
- 出典データセット
- uspto-grants-2004_03
- 特許番号
- US06706725B1
関連ノート
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