化工社化工社 化学情報印刷レポート · 研究参考用
Thioxanthone → 9H-thioxanthen-9-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thioxanthone | HCID 10295 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 9H-thioxanthen-9-ol | HCID 5154170 | 93% |
反応手順
A suspension of thioxanthen-9-one [31] (2 g, 9.42 mmol) in anhydrous CH3OH (30 mL) was stirred under N2 and NaBH4 (1.42 g, 37.68 mmol) was added slowly in portions over 15 min. After complete addition the reaction mixture was heated at reflux (3 hr.) and cooled to room temperature. Ice-water was added and the reaction mixture was extracted with CH2Cl2 (3×50 mL). The combined CH2Cl2 extracts were washed with water, brine, dried (MgSO4). The solvent was removed under reduced pressure to give a yellow solid, which was recrystallized from pet.ether to give 1.87 g (93%) of the alcohol as pale yellow needles, mp 104-105° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06806283B2 |
| 出典データセット | uspto-grants-2004_10 |
| ORD ID | ord-5a0f4c1e54344c8ca6ce20442184321b |
| 出典メモ | uspto-grants-2004_10 |