化工社化工社 化学情報印刷レポート · 研究参考用
Bromine → 4-bromo-9a-butyl-8-chloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 9a-butyl-8-chloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one | HCID 21990923 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-bromo-9a-butyl-8-chloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one | HCID 21990872 | — |
反応手順
A solution of 9a-butyl-8-chloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one (555 mg, 1.82 mmol) in anhydrous dichloromethane (18.2 mL) was treated with sodium bicarbonate (765 mg, 9.1 mmol) and bromine (0.093 mL, 1.82 mmol). The mixture was stirred at room temperature for 30 minutes and then diluted with CH2Cl2 (50 mL) and washed with water (50 mL). The organic phase was dried over MgSO4, filtered through a pad of silica gel (10 mL) with a 10 mL CH2Cl2 rinse, and the solvent evaporated under vacuum. The residue (0.55 g) was lyophilized from benzene to afford 4-bromo-9a-butyl-8-chloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one as an amorphous solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07087599B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-9cf6287b0a4c41f28bee99b9776571b1 |
| 出典メモ | uspto-grants-2006_08 |