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Potassium Carbonate → 4-[(4-Methylphenyl)sulfonyl]-9-nitro-3,4,5,6-tetrahydro-2H-1,7,4-benzodioxazonine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | N,N-bis(2-(p-toluenesulfonyloxy)ethyl)-p-toluenesulfonamide | HCID 267409 | — |
| 反応物 | 4-Nitrocatechol | HCID 3505109 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-[(4-Methylphenyl)sulfonyl]-9-nitro-3,4,5,6-tetrahydro-2H-1,7,4-benzodioxazonine | HCID 14856355 | — |
反応手順
To dimethylformamide (200 mL) add 4-nitrocatechol (13.8 g, 89 mmol), 4-methyl-N,N-bis[2-[[(4-methylphenyl)sulfonyl]oxy]ethyl]benzenesulfonamide (50.7 g, 89.4 mmol), and K2CO3 (27 g, 0.19 mol). Stir and heat the reaction at 110° C. Monitor the progress of the reaction by thin-layer chromatography. Upon completion remove the heat and add water (1.3 L) and methanol (300 mL). Collect the precipitate on paper by suction filtration. Wash the solid with water (2 L). Chromatograph the material on silica (300 g) with CH2Cl2 to obtain the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04966967 |
| 出典データセット | uspto-grants-1990_10 |
| ORD ID | ord-b8b68b4a029d40cca1a79aeddaa89174 |
| 出典メモ | uspto-grants-1990_10 |