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Benzamide, 2-(aminosulfonyl)-N,N-diethyl-4-methoxy-6-(1-methylethyl)- → 4-Isopropyl-6-methoxysaccharin
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzamide, 2-(aminosulfonyl)-N,N-diethyl-4-methoxy-6-(1-methylethyl)- | HCID 10336632 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 4-Isopropyl-6-methoxysaccharin | HCID 10147362 | 91% |
反応手順
A solution of 2.aminosulfonyl-6-isopropyl-4-methoxy-N,N-diethylbenzamide (429.6 g) in acetic acid (1.5 L) was refluxed for 20 hours, then cooled to room temperature. The solvent was removed under vacuum. The oily residue was dissolved in water (6 L) and the pH was adjusted to 1 with hydrochloric acid (6N). The crude product was collected by filtration, washed with water (2 L), dried at 60° C. under vacuum for 18 hours and recrystallized from ethyl acetate-hexane to give 4-isopropyl-6-methoxysaccharin (303 g, 91% yield, m.p. 188° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05466701 |
| 出典データセット | uspto-grants-1995_11 |
| ORD ID | ord-0a8197a401934a08a1fab500f722f634 |
| 出典メモ | uspto-grants-1995_11 |