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Chloroform → 2-Bromo-9,10-dihydro-1-thiabenzo[f]azulen-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | 9,10-Dihydro-4H-benzo[4,5]cyclohepta[1,2-b]thiophen-4-one | HCID 768492 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Bromo-9,10-dihydro-1-thiabenzo[f]azulen-4-one | HCID 67167626 | 69.5% |
反応手順
Bromine (8.5 mL, 165 mmol) was added dropwise to a chloroform (300 mL) solution of 9,10-dihydro-1-thiabenzo[f]azulen-4-one (23.2 g, 108 mmol), and the mixture was stirred for 4 hours. Water was added to the reaction mixture, the product was extracted with ethyl acetate, the organic layer was then washed with a saturated aqueous sodium bicarbonate solution and with a saturated sodium chloride solution, and dried over anhydrous sodium sulfate. The solvents were distilled off under a reduced pressure, and the residue was purified by silica gel chromatography (hexane-ethyl acetate), to give 22.0 g (69%) of the captioned compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08377967B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-32bf708a922040b59afc2e4d63b8cc8d |
| 出典メモ | uspto-grants-2013_02 |