反応式
[CH3:1]C(C)([O-])C.[K+].[O:7]1[CH2:12][CH2:11][CH2:10][O:9][CH:8]1[CH2:13][CH2:14][O:15][C:16]1[CH:23]=[CH:22][C:19]([CH:20]=O)=[CH:18][CH:17]=1>[Br-].C[P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.CCOCC>[CH:20]([C:19]1[CH:22]=[CH:23][C:16]([O:15][CH2:14][CH2:13][CH:8]2[O:9][CH2:10][CH2:11][CH2:12][O:7]2)=[CH:17][CH:18]=1)=[CH2:1]参加物
実験手順
In another 2 liter flask, 57.2 g of methyl triphenylphosphonium bromide was placed. 500 ml of anhydrous ether was poured and then, stirred. To the resulting solution was slowly added 18.0 g of potassium tert-butoxide and reacted at room temperature for 3 hrs. 25.6 g of the above 4-(2-[1,3]-dioxane-2-yl-ethoxy)benzaldehyde was dissolved in 200 ml of anhydrous ether and was slowly added to the reaction mixture and then subjected to reaction at room temperature for 4 hrs. After completion of the reaction, the produced solid by-product was filtered off and washed with distilled water and saturated saline. The organic phase washed was dried over anhydrous magnesium sulfate and the solvent was removed by distillation under reduced pressure. The reaction mixture was purified by Silica gel column chromatography to obtain 19.7 g of 2-[2-(4-vinylphenoxy)ethyl]-[1,3]-dioxane, represented by the following formula: ##STR9##
後処理
- customreacted at room temperature for 3 hrs
- additionwas slowly added to the reaction mixture
- customsubjected to reaction at room temperature for 4 hrs
- customAfter completion of the reaction
- filtrationthe produced solid by-product was filtered off
- washwashed with distilled water and saturated saline
- washThe organic phase washed
- dry with materialwas dried over anhydrous magnesium sulfate
- customthe solvent was removed by distillation under reduced pressure
- customThe reaction mixture was purified by Silica gel column chromatography
出典と根拠
- ORDレコード
- ord-7962a8e3cbfa49e3aabf54e37edc9672
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05723258
関連ノート
読み込み中…