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Sodium hydride → 2-Nitro-N-[3-(3-oxo-2,3-dihydrocyclopenta[c]carbazol-6(1H)-yl)propyl]-N-propylbenzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Ethyl acetate hexane | HCID 21226206 | — |
| 反応物 | 1,6-Dihydrocyclopenta[c]carbazol-3(2H)-one | HCID 58544896 | — |
| 反応物 | N-(3-bromopropyl)-2-nitro-N-propylbenzenesulfonamide | HCID 67368759 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Nitro-N-[3-(3-oxo-2,3-dihydrocyclopenta[c]carbazol-6(1H)-yl)propyl]-N-propylbenzenesulfonamide | HCID 67377946 | — |
反応手順
Compound 46 (0.538 g, 2.43 mmol) and bromide 50 (0.9 g, 2.46 mmol) were dissolved in CH2Cl2 (30 mL). Then NaH (0.15 g, 3.75 mmol, 1.5 eq.) was added. The reaction mixture was stirred for 20 min (TLC monitoring, eluent: hexane-ethyl acetate, 1:1). Then, the mixture was poured onto ice. The product was extracted with ethyl acetate, and the extract was evaporated in a rotary evaporator. The residue of CH2Cl2 was removed in high vacuum. Methanol was added to the hardened precipitate. The product was triturated; the precipitate was filtered off. Yield of 47: 0.638 g (52%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09108916B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-77464d43f4d142cab6f2ff4bb888b4b6 |
| 出典メモ | uspto-grants-2015_08 |