関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | (+)-Narwedine | HCID 441596 | — |
| 反応物 | Lithium tri-s-butylborohydride | HCID 3611392 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Galantamine, (+)- | HCID 906210 | — |
反応手順
2 mmole (1N in tetrahydrofuran {THF}) of L-Selectride® (lithium tri-sec-butylborohydride, Aldrich) is charged into 8 ml THF and cooled to -78° C. 1 mmole of (+)-narwedine in 50 ml THF is added dropwise over a period of 30 minutes. After addition, the solution is stirred at -78° C. for 2 hours and then warmed to 0° C. 0.4 ml of methanol is added and the solution is warmed to 25° C. and stirred for 15 minutes. Solvent is then evaporated under vacuum to dryness to obtain a syrup. The syrup is dissolved in 0.5 ml CHCl3 and the solution is loaded into a SiO2 200-400 mesh, 6A, column. The column is eluted with a solvent mixture of CH2Cl2 /CH3OH 6:1 to obtain pure (+)-galanthamine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05428159 |
|---|
| 出典データセット | uspto-grants-1995_06 |
|---|
| ORD ID | ord-776d92d9740843baac2ed5cc2f7eae00 |
|---|
| 出典メモ | uspto-grants-1995_06 |
|---|