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Hydrochloric Acid → 1-[3-[[1-[3-(Aminosulfonyl)-4-chlorophenyl]2,3-dihydro-3-oxo-1H-isoindol-1yl]thio]-2-methyl-1-oxopropyl]-L-proline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Chlorthalidone | HCID 2732 | — |
| 反応物 | 1-(2-Methyl-3-sulfanylpropanoyl)-L-proline | HCID 12877547 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-[3-[[1-[3-(Aminosulfonyl)-4-chlorophenyl]2,3-dihydro-3-oxo-1H-isoindol-1yl]thio]-2-methyl-1-oxopropyl]-L-proline | HCID 13022693 | 48.4% |
反応手順
A mixture of 1.69 g chlorthalidone, 2.5 g of 1-(3-mercapto-2-methyl-1-oxopropyl)-L-proline and 150 ml ethyl acetate is cooled by an ice bath and then saturated with HCl gas. This mixture is refluxed for one hour. The solvent is evaporated, the residue dissolved in warm saturated sodium bicarbonate solution, and the mixture extracted with ethyl acetate. The aqueous phase is separated and acidified at ice bath temperature. The resulting solid is filtered off, washed with water and dried to yield 1.3 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04312809 |
| 出典データセット | uspto-grants-1982_01 |
| ORD ID | ord-3487d77bc92d42d49d7493b3acae8727 |
| 出典メモ | uspto-grants-1982_01 |