化工社化工社 化学情報印刷レポート · 研究参考用
Sodium borohydride → Npc182939
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | Qing Hau Sau | HCID 9838675 | — |
| 反応物 | Acetic acid methanol | HCID 10129899 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Npc182939 | HCID 456410 | 75% |
反応手順
Artemisinin (compound 3) (0.5 g, 1.8 mmole) in 40 mL of MeOH was cooled in an ice-bath to 0°-5° C. To the solution was added in small portions 0.25 g (6.6 mmole) of NaBH4 over a period of 30 minutes. The solution was stirred at 0°-5° C. for 2 hours after the addition of NaBH4 was complete. The solution was neutralized with 30% AcOH/MeOH and evaporated to dryness under reduced pressure. The white residue was extracted 3 times with 50 mL of EtOAc. The EtOAc extracts were combined, filtered, and evaporated to dryness to give 0.38 g (75%) of white needles mp 152°-154° C. (dec). Recrystallization from EtOAc-hexane raised the melting point to 153°-155° C. (lit. mp 153°-154° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04791135 |
| 出典データセット | uspto-grants-1988_12 |
| ORD ID | ord-42dfb6d64921409b843d06906f4bf799 |
| 出典メモ | uspto-grants-1988_12 |