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Diisopropyl Ether → Ethyl 2-(4-Chlorophenyl)-5,5-diphenyl[1,3]-dioxane-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropyl Ether | HCID 7914 | — |
| 反応物 | Boron trifluoride etherate | HCID 8000 | — |
| 反応物 | 2,2-Diphenylpropane-1,3-diol | HCID 410445 | — |
| 反応物 | Ethyl 4-chlorobenzoylformate | HCID 2758815 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | Ethyl 2-(4-Chlorophenyl)-5,5-diphenyl[1,3]-dioxane-2-carboxylate | HCID 15428824 | 71% |
反応手順
42.5 g (0.2 M) of ethyl 2-oxo-2-(4-chlorophenyl)acetate are placed in 400 ml of CH2Cl2 in a 500 ml reactor. 22.8 g (0.1 M) of 2,2-diphenylpropane-1,3-diol and then 14.2 g (0.1 M) of BF3.Et2O are added. The mixture is left to react with stirring for 72 h at room temperature. The reaction mixture is taken up in NaHCO3 solution. The organic phase is washed with saturated NaCl solution. After drying over Na2SO4 and concentration, a very thick oil is obtained. 150 ml of isopropyl ether are added and a white precipitate forms. After filtration, 30 g of product melting at 156-158° C. are obtained (yield: 71%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06528538B1 |
| 出典データセット | uspto-grants-2003_03 |
| ORD ID | ord-2169fac0a9014699bb9176b535bf9222 |
| 出典メモ | uspto-grants-2003_03 |