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Piperidine → Acemetacin
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Allyl 1-(4-chlorobenzoyl)-5-methoxy-2-methyl-3-indoleacetoxyacetate | HCID 13654465 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Acemetacin | HCID 1981 | — |
反応手順
31.9 g of acemetacin allyl ester, 100 ml of toluene, 2.3 g of triphenylphosphine and 0.75 g of palladium on charcoal (5% strength) are taken as an initial charge, under nitrogen. 11.9 g of piperidine are added dropwise, with stirring, and the mixture is then stirred for a further 3 hours at 90° C. It is filtered hot and the catalyst is rinsed with hot toluene. The filtrate is evaporated, the residue is taken up in methylene chloride (about 300 ml) and this solution is washed with half-concentrated hydrochloric acid (100 ml) and then with water. After removal of the solvent in vacuo, the residue is recrystallized from toluene.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04658039 |
| 出典データセット | uspto-grants-1987_04 |
| ORD ID | ord-86f99fbf4277483ca14ccb71c12ba64b |
| 出典メモ | uspto-grants-1987_04 |