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2-Chlorobenzenesulfonyl chloride → 2-Chloro-N-[4-(7,8-dimethoxy-1-oxo-2,2a,4,5-tetrahydro-1H-3-aza-acenaphthylen-3-yl)-butyl]-benzenesulfonamide hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Chlorobenzenesulfonyl chloride | HCID 76187 | — |
| 反応物 | 3-(4-Amino-butyl)-7,8-dimethoxy-2a,3,4,5-tetrahydro-2H-3-aza-acenaphthylen-1-one dihydro-chloride | HCID 67358582 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Chloro-N-[4-(7,8-dimethoxy-1-oxo-2,2a,4,5-tetrahydro-1H-3-aza-acenaphthylen-3-yl)-butyl]-benzenesulfonamide hydrochloride | HCID 44123943 | 119% |
反応手順
2-Chlorobenzenesulfonyl chloride (92.4 mg, 0.44 mmol) was added to a solution of 3-(4-Amino-butyl)-7,8-dimethoxy-2a,3,4,5-tetrahydro-2H-3-aza-acenaphthylen-1-one dihydro-chloride (150 mg, 0.40 mmol) and NN′-diisopropylethylamine (0.400 ml) in CH2Cl2 (20 mL) and the mixture was stirred overnight at room temperature. The resulting solution was washed with water (3×20 mL), dried over Na2SO4 and evaporated to dryness. The free base was dissolved in ethyl acetate (2 ml) and A 2.8 M solution of hydrogen chloride in ethanol was then added. The product was crystallized and collected by filtration, and vacuum dried to give a pale brown solid (135 mg, 66%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07553965B2 |
| 出典データセット | uspto-grants-2009_06 |
| ORD ID | ord-cbf001c4f4e54891a77d2280ca5044cd |
| 出典メモ | uspto-grants-2009_06 |