関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Sodium Bisulfite | HCID 23665763 | — |
| 反応物 | Potassium hydroxy sulfite | HCID 23707502 | — |
| 反応物 | 5-Bromo-1,3-dihydro-2-benzothiophene | HCID 59801489 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5-Bromo-1,3-dihydro-benzo(c)thiophene 2,2-dioxide | HCID 288396 | 65% |
反応手順
Dissolve 5-bromo-1,3-dihydro-benzo[c]thiophene (1.25 g, 5.79 mmol) in methanol (25 mL) and add oxone (10.7 g, 17.4 mmol). Stir the reaction mixture for 2 hours at 0° C. and then add a 1M aqueous sodium bisulfite solution (100 mL). Stir the reaction mixture for 10 minutes and add saturated NaHCO3 solution (200 mL). Extract the aqueous layer with CH2Cl2 (3×100 mL). Combine the organic layers and dry with Na2SO4, filter, concentrate and purify by flash column chromatography (silica gel, 0-5% MeOH/CH2Cl2) to give 930 mg of 5-bromo-1,3-dihydro-benzo[c]thiophene 2,2-dioxide 65%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07585977B2 |
|---|
| 出典データセット | uspto-grants-2009_09 |
|---|
| ORD ID | ord-7c085e5eaa9c4274a1e99e22f1d16ac9 |
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| 出典メモ | uspto-grants-2009_09 |
|---|
