関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Isopropanol | HCID 3776 | — |
| 反応物 | Furylacrylic acid | HCID 10876 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Propenoic acid, 3-(2-furanyl)-, 1-methylethyl ester | HCID 909932 | 96% |
反応手順
1.46 ml of thionyl chloride (20 mmol) were added to a solution of 1.38 g of 3-(2-furyl)acrylic acid (10 mmol) in 10 ml of chloroform and 0.1 ml of DMF. The solution was warmed to 70° C. and kept at this temperature for 1 h, then the solvents were removed under reduced pressure and the residue was dissolved in 6.6 ml of DCM and 3.3 ml of pyridine and subsequently cooled to 0° C. 0.96 ml of 2-propanol (12.5 mmol) was added, the temperature was increased to RT and the reaction mixture was stirred for 2.5 h. It was acidified with 30 ml of 1 M hydrochloric acid and extracted with 150 ml of ethyl acetate. The organic phase was washed with aqueous sodium hydrogencarbonate solution, dried over sodium sulfate, filtered and the solvents were removed under reduced pressure. 1.72 g (yield: 96%) of the title compound were obtained. LC/MS (Method D) (M+H-isopropyl)+ 139
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08097758B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-9be70656195b4bdda623c09e30b4d6b4 |
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| 出典メモ | uspto-grants-2012_01 |
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