化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → HCID 20528316、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Benzoin | HCID 8400 | — |
| 反応物 | Piperonal | HCID 8438 | — |
| 反応物 | Potassium Cyanide | HCID 9032 | — |
| 反応物 | 4-Fluorobenzaldehyde | HCID 68023 | — |
| 反応物 | 1,3-Diazepane-2-thione | HCID 736589 | — |
| 反応物 | HCID 54204893 | HCID 54204893 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 20528316 | HCID 20528316 | — |
反応手順
A mixture consisting of 12 g. of piperonal 8.4 ml. of p-fluorobenzaldehyde, 6 g. of potassium cyanide, and 80 ml. of 65% ethanol is reacted as described in Example 20, giving 11.7 g. of 4'-fluoro-3,4-methylenedioxybenzoin as an uncrystallizable oil. 9.0 g. of this benzoin is converted to its methanesulfonate ester by the procedure of Example 20, yielding 9.8 g. of ester as an uncrystallizable oil. The reaction of 4.9 g. of the crude methanesulfonate ester, and 1.16 g. of hexahydro-2H-1,3-diazepin-2-thione in 80 ml. of acetone, followed by treatment with 5 ml of 2 N ethanolic hydrogen chloride gives the title compound melting at 211°-213° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04344954 |
| 出典データセット | uspto-grants-1982_08 |
| ORD ID | ord-ba8adce569ad490c9586f19986e695ad |
| 出典メモ | uspto-grants-1982_08 |