関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | Methyl 4-amino-1H-indole-6-carboxylate | HCID 14243967 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 4-[(methylsulfonyl)amino]-1H-indole-6-carboxylate | HCID 21086208 | 50.5% |
反応手順
To a mixture of methyl 4-amino-1H-indole-6-carboxylate (1.0 g) in DMF (10 mL) was added 4-dimethylaminopyridine (1.46 g) and methanesulfonyl chloride (0.6 g). The mixture was heated to 60° C. for 3 h, cooled to room temperature, and partitioned between water and ethyl acetate. The layers were separated and the organic layer washed three times with brine, dried over anhydrous sodium sulfate and concentrated to give 0.71 g of the title compound: 1H NMR (CDCl3) δ 3.02, 3.94, 6.69, 7.42, 7.81, 8.04.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07727997B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-af7cd9f759014a5f8832d2a50b3f6f11 |
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| 出典メモ | uspto-grants-2010_06 |
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