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Hydrochloric Acid → N-(2-[N-(2-benzyloxy-5-bromobenzyl)-N-ethylamino]pyridine-5-carbonyl)propanesulphonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Dimethylaminopyrimidine | HCID 521717 | — |
| 反応物 | Propane-1-sulphonamide | HCID 3401849 | — |
| 反応物 | 2-[N-(5-bromo-2-benzyloxybenzyl)-N-ethylamino]pyridine-5-carboxylic acid | HCID 11351190 | — |
| 反応物 | 1-(3-Dimethylaminopropyl)ethylcarbodiimide hydrochloride | HCID 21982921 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(2-[N-(2-benzyloxy-5-bromobenzyl)-N-ethylamino]pyridine-5-carbonyl)propanesulphonamide | HCID 22105639 | 24.6% |
反応手順
To a solution of 2-(N-(2-benzyloxy-5-bromobenzyl)-N-ethylamino]pyridine-5-carboxylic acid (0.89 g) in dichloromethane (50 ml) was added propanesulphonamide (0.3 g), dimethylaminopyrimidine (0.493 g) and 1-(3-dimethylaminopropyl)ethylcarbodiimide hydrochloride (0.58 g). The mixture was stirred at ambient temperature for 18 hours, and poured into 2N HCl. The organic layer was separated and washed with water and brine, then dried (MgSO4), filtered and evaporated. The resulting oil was purified by chromatography on silica gel (eluting with 5% ethylacetate/dichloromethane to give N-(2-[N-(2-benzyloxy-5-bromobenzyl)-N-ethylamino]pyridine-5-carbonyl)propanesulphonamide (271 mg) as a white foam.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05843942 |
| 出典データセット | uspto-grants-1998_12 |
| ORD ID | ord-8c64db4ba7724ab8abb4c242bc02427f |
| 出典メモ | uspto-grants-1998_12 |