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Hydrochloric Acid → Acemetacin
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | Allyl 1-(4-chlorobenzoyl)-5-methoxy-2-methyl-3-indoleacetoxyacetate | HCID 13654465 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Acemetacin | HCID 1981 | — |
反応手順
0.003 mole of tetrakis-triphenylphosphine-palladium-(O) is added to 0.03 mole of acemetacin allyl ester in 50 ml of tetrahydrofuran, under nitrogen. 0.3 mole of piperidine is added dropwise at 20°-25° C., with stirring, and stirring is then continued for 2 hours at room temperature (check by thin layer chromatography). 200 ml of half-concentrated hydrochloric acid are added dropwise with cooling, the phases are separated off, the aqueous phase is extracted twice with methylene chloride and the combined organic phases are evaporated in vacuo. The residue is recrystallised 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-f58d4d42e84347c99776474a7ff89b38 |
| 出典メモ | uspto-grants-1987_04 |