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Propane sultone → 1,2,3,4-Tetrahydroquinoline-N-propanesulphonic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Propane sultone | HCID 14264 | — |
| 反応物 | 1,2,3,4-Tetrahydroquinoline | HCID 69460 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1,2,3,4-Tetrahydroquinoline-N-propanesulphonic acid | HCID 9249739 | — |
反応手順
48.8 molten propane-1,3-sultone were added dropwise at 60+ to 80° C. within the course of 50 minutes to 58.4 g 1,2,3,4-tetrahydroquinoline in a 500 ml. flask. The reaction mixture was left for 3.45 hours at about 70° C. and subsequently 470 ml. methanol were added portionwise under reflux conditions and further stirred under reflux conditions until the solid, glasslike under material had dissolved completely. Thereafter, the reaction mixture was cooled to ambient temperature, while stirring, a rapid crystallization thereby taking place. After leaving to stand for about 12 hours in a refrigerator, the crystals were filtered off. Yield about 50 g.; m.p. 233°-237° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04845030 |
| 出典データセット | uspto-grants-1989_07 |
| ORD ID | ord-a5d6c7e92cdf434286cb8502d02db8d3 |
| 出典メモ | uspto-grants-1989_07 |