関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Stannous Chloride | HCID 24479 | — |
| 反応物 | 1-Chloro-6-methyl-5-nitroisoquinoline | HCID 22622221 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Dichloromethane ethanol | HCID 21584144 | — |
| 生成物 | 1-Chloro-6-methylisoquinolin-5-amine | HCID 59627375 | 40.4% |
反応手順
Tin (II) chloride (0.43 g, 2.2 mmol) was added to a solution of 1-chloro-6-methyl-5-nitroisoquinoline (0.100 g, 0.45 mmol) in ethanol/DCM (10.0 mL, 4:1). The solution was heated at 70° C. for 16 h. The reaction mixture was diluted with DCM and the organic phase was washed with saturated aqueous sodium bicarbonate solution and brine, dried over anhydrous sodium sulfate, filtered, and concentrated to afford a brown solid which was purified via column chromatography on silica gel (RediSep 40 g column, gradient elution with 0-50% ethyl acetate-hexane) to afford 1-chloro-6-methylisoquinolin-5-amine (0.035 g, 40% yield) as a brown solid. MS (ESI, pos. ion) m/z: 193 [M+H]+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08557830B2 |
|---|
| 出典データセット | uspto-grants-2013_10 |
|---|
| ORD ID | ord-d8de82e3eeb9429bb135be4b66ab8ddd |
|---|
| 出典メモ | uspto-grants-2013_10 |
|---|