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Hydrochloric Acid → 4'-(3-(1-Pyrrolidinyl)propionyl)methanesulfonanilide hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Pyrrolidine, hydrochloride (1:1) | HCID 212848 | — |
| 反応物 | N-(4-acetylphenyl)methanesulfonamide | HCID 684083 | — |
| 触媒 | Ethanol | HCID 702 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4'-(3-(1-Pyrrolidinyl)propionyl)methanesulfonanilide hydrochloride | HCID 3042693 | — |
反応手順
A mixture of 4'-acetylmethanesulfonanilide (21.5 g., 0.1 mole), 95% paraformaldehyde (10 g., 0.3 mole), pyrrolidine hydrochloride (10.8 g., 0.1 mole) in 150 ml. of ethanol containing 1 drop of concentrated hydrochloric acid is refluxed for a period of 4 hr. at steam bath temperature and then for an additional period of 8 hr. permitting the ethanol to evaporate. The resulting glassy residue is stirred with 300 ml. of hot acetone providing a crystalline material which is collected and crystallized from methanol-isopropyl alcohol to afford analytically pure 4'-[3-(1-PYRROLIDINYL)PROPIONYL]-METHANESULFONANILIDE HYDROCHLORIDE, m.p. 182.0°-183.0°C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03968242 |
| 出典データセット | uspto-grants-1976_07 |
| ORD ID | ord-e567233c2e9e45eba084244edecee822 |
| 出典メモ | uspto-grants-1976_07 |