関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 2-Nitrophenol | HCID 6947 | — |
| 反応物 | Triethyl orthoacetate | HCID 66221 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Ethyl 2-(furan-2-yl)acetate | HCID 11252124 | 377.8% |
反応手順
A solution of 60.8 g (0.4 mole) of the carbinol obtained according to letter (a) above, 11.1 g (0.08 mole) of o-nitro-phenol and 194.4 g (1.2 mole) of triethyl ortho-acetate were slowly heated during 8-10 h to 145°-150° under nitrogen atmosphere while stirring. Meanwhile, ethanol and ethyl acetate formed in the course of the reaction were gradually distilled off whereas the excess of triethyl ortho-acetate was recovered by vacuum distillation. The thus obtained residue was dissolved in petrol ether (b.p. 30°-50°) and the resulting solution was washed with 5% aqueous NaOH, dried over Na2SO4 and finally evaporated. 46.6 g (yield 52.5%) of the title ethyl furyl-acetate were obtained by fractional distillation. Purity ca. 35%; b.p. 65°-70°/0.2 Torr.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04203907 |
|---|
| 出典データセット | uspto-grants-1980_05 |
|---|
| ORD ID | ord-58948c495ced47a495abaf2fa0bbebdb |
|---|
| 出典メモ | uspto-grants-1980_05 |
|---|