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Benzenesulfonyl chloride → N,N-bisbenzenesulfonyl-(4-bromo-2-iodoaniline)
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzenesulfonyl chloride | HCID 7369 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Bromo-2-iodoaniline | HCID 823934 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | N,N-bisbenzenesulfonyl-(4-bromo-2-iodoaniline) | HCID 60026850 | 35% |
反応手順
A solution of 4-bromo-2-iodoaniline (8.5 g, 28.5 mmol) in 200 mL of dichloromethane was sequentially treated with benzenesulfonyl chloride (15 mL, 117.5 mmol) and triethylamine (25 mL, 179.6 mmol). After 4 days, the mixture was diluted with 100 mL of saturated aqueous sodium bicarbonate solution and extracted with three 100 mL portions of ethyl acetate. The combined organic layers were washed with 50 mL of brine, three 60 mL portions of saturated aqueous ammonium chloride solution, dried over magnesium sulfate, filtered, and concentrated in vacuo. The crude product was triturated with diethyl ether to afford 5.74 g (35% yield) of N,N-bisbenzenesulfonyl-(4-bromo-2-iodoaniline).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08741897B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-53ca051e0a414058a5925be0c353bd28 |
| 出典メモ | uspto-grants-2014_06 |