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Dichloromethane → Methyl 2-{[(4,5,6-trimethylpyrimidin-2-yl)aminocarbonyl]aminosulfonyl}benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Benzoic acid, 2-(isocyanatosulfonyl)-, methyl ester | HCID 156281 | — |
| 反応物 | 4,5,6-Trimethylpyrimidin-2-amine | HCID 12250862 | — |
| 溶媒 | Butyl Chloride | HCID 8005 | — |
| 生成物 | Methyl 2-{[(4,5,6-trimethylpyrimidin-2-yl)aminocarbonyl]aminosulfonyl}benzoate | HCID 13038388 | — |
反応手順
To a mixture of 1.0 gram (0.0073 mole) of 2-amino-4,5,6-trimethylpyrimidine and 5.0 ml of dried methylene chloride stirring magnetically in a 50 ml RB single neck flask, 2.1 grams of methyl 2-(isocyanatosulfonyl)benzoate was added at room temperature and the mixture stirred at room temperature for 24 hours. Butyl chloride (4 ml) was added with constant stirring and the insoluble product filtered, washed immediately with butyl chloride and dried. (Yield 1.3 grams, m.p. 152°-161°). IR (Nujol): 5.60, 5.75 (C=O), 11.25 11.90 microns; NMR (TFA-d): δ2.30 (s,3H,CH3), 2.65 (s, 6H, 2CH3), 4.00 (s, 3H, CO2CH3), 7.60-8.60 (m, ArH).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04342587 |
| 出典データセット | uspto-grants-1982_08 |
| ORD ID | ord-d5dab4561c9d452a95c1e193556c737d |
| 出典メモ | uspto-grants-1982_08 |