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Hydrochloric Acid → Methyl 4-(N-(benzofuran-5-ylmethyl)sulfamoyl)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1-Benzofuran-5-ylmethylamine | HCID 2795182 | — |
| 反応物 | Methyl 4-(Chlorosulfonyl)benzoate | HCID 4738388 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl 4-(N-(benzofuran-5-ylmethyl)sulfamoyl)benzoate | HCID 66837840 | 55% |
反応手順
To a solution of benzofuran-5-ylmethanamine (6.5 g, 28 mmol) in DCM (100 mL) was added methyl 4-(chlorosulfonyl)benzoate (4.1 g, 28 mmol) in portion wise at 0° C., and the mixture was stirred at room temperature for 3 hrs. The mixture was added 2 M aqueous HCl (80 mL) to give a white suspension. A half volume of DCM was removed by nitrogen flow, and the precipitates were collected by filtration, washed with water, and the solid was dried in vacuo at 50° C. to give 5.3 g (55% yield) of the titled compound as a off-white solid. The filtrate formed a suspension, which was collected by filtration, washed with water, and the solid was dried in vacuo at 50° C. to give 3.4 g (35% yield) of the titled compound as a pale brown white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08829026B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-d6962fdbf85542c599111db05d8ec0f7 |
| 出典メモ | uspto-grants-2014_09 |