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Benzene, 1,2-dimethoxy-4-(2-nitroethyl)- → 1-(3',4'-Dimethoxyphenyl)-7-phenyl-2-nitro-5-heptanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzene, 1,2-dimethoxy-4-(2-nitroethyl)- | HCID 10036050 | — |
| 反応物 | 1-Iodo-5-phenyl-3-pentanone | HCID 20164202 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(3',4'-Dimethoxyphenyl)-7-phenyl-2-nitro-5-heptanone | HCID 20164219 | 113.2% |
反応手順
To a solution of 36 g (0.17 mole) of 2-(3,4-dimethoxyphenyl)-1-nitroethane in 300 mL of dry tetrahydrofuran was added 71 g (0.17 mole) of 40% Triton B. The solution was stirred at room temperature for 10 min. 55.3 g (0.19 mole) of 1-iodo-5-phenyl-3-pentanone in a minimum amount of dry tetrahydrofuran was added dropwise. The mixture was stirred at room temperature for 30 min, at 50° C. for 3 hr., then allowed to stir at room temperature overnight. Solvent was removed in vacuo and the residue taken up in ether and extracted twice with water. The organic layer was dried over anh Mg SO4, and concentrated at reduced pressure to give 71.5 g of crude oil. This crude material was passed through HPLC to give 46.4 g. of purified material.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04342692 |
| 出典データセット | uspto-grants-1982_08 |
| ORD ID | ord-c067a0383e4d4285a429c03fc770b411 |
| 出典メモ | uspto-grants-1982_08 |