関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Benzo(b)thiophene-2-carboxylic acid | HCID 95864 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 6,6-Difluoro-5-methyl-5-hexenyl methanesulfonate | HCID 23020371 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 6,6-Difluoro-5-methyl-5-hexenyl benzo[b]thiophene-2-carboxylate | HCID 69181690 | 81% |
反応手順
To 40 ml of N,N-dimethylformamide were dissolved 5.00 g (22 mmol) of 6,6-difluoro-5-methyl-5-hexenyl methanesulfonate and 4.30 g (24 mmol) of benzo[b]thiophene-2-carboxylicacid, followed by the addition of 6.00 g (71 mmol) of sodium hydrogencarbonate and stirring at 100° C. for 3 hours. The reaction liquid was then poured in water and extracted with diethyl ether. The organic layer was washed with water and a saturated saline solution in this order, followed by drying over anhydrous magnesium sulfate and concentration under reduced pressure. The residue was purified with silica gel column chromatography (diisopropyl ether:hexane=1:7) to obtain 5.50 g (yield: 81%) of 6,6-difluoro-5-methyl-5-hexenyl benzo[b]thiophene-2-carboxylate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07273878B2 |
|---|
| 出典データセット | uspto-grants-2007_09 |
|---|
| ORD ID | ord-9db6e71ddd914462931406307e242912 |
|---|
| 出典メモ | uspto-grants-2007_09 |
|---|