関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphoric Acid | HCID 1004 | — |
| 反応物 | Venlafaxine | HCID 5656 | — |
| 反応物 | Sodium benzenethiol | HCID 66586497 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Desvenlafaxine | HCID 125017 | — |
反応手順
Venlafaxine (5.6 g) and benzenethiol sodium salt (6.9 g) are charged to PEG 400 (25 g). The reaction mixture is heated to 160° C. for 5 hours. Then the temperature is lowered and water is added (60 g). The pH is adjusted to 3.5 with H3PO4. The organic by-products are removed by extraction with heptanes (25 g). The pH of the aqueous layer is then adjusted to 9.5 with aqueous ammonia. The precipitate is collected by suction filtration, re-slurried in water (100 g), isolated by suction filtration and dried in vacuo.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07154001B2 |
|---|
| 出典データセット | uspto-grants-2006_12 |
|---|
| ORD ID | ord-45fafbe0bbc64b9b947cd0b54ba8fe40 |
|---|
| 出典メモ | uspto-grants-2006_12 |
|---|
