関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 6-Methoxy-1-benzothiophene | HCID 13634237 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | 2-Bromo-6-methoxybenzo[b]thiophene | HCID 23512902 | 82.2% |
反応手順
N-bromosuccinimide (14.70 g, 82.59 mmol) and p-toluenesulfonic acid (2.70 g, 15.68 mmol) were added to a solution of benzothiophene (3) (15.10 g, 92.07 mmol) in 1,2-dichloroethane (300 ml). The mixture was maintained at 70° C. for 35 min, cooled in an ice bath, and the succinimide was removed by filtration. The solution was extracted with saturated sodium bicarbonate solution, dried over Na2SO4, filtered, and concentrated under vacuum to give 22.00 g as an oil. Crystallisation from pentane afforded a white solid (16.50 g, 74%), mp 62° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07476691B2 |
|---|
| 出典データセット | uspto-grants-2009_01 |
|---|
| ORD ID | ord-77fd94c4c66d4329b9c479b4e8728942 |
|---|
| 出典メモ | uspto-grants-2009_01 |
|---|