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Hydrochloric Acid → N-[(4,6-Dimethylpyrimidin-2-yl)aminocarbonyl]-3-methyl-2-pyridinesulfonamide-1-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Amino-4,6-dimethyl pyrimidine | HCID 13021 | — |
| 反応物 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 反応物 | 3-Methylpyridine-2-sulfonamide | HCID 12295469 | — |
| 反応物 | Phenylcarbamate | HCID 21896570 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | N-[(4,6-Dimethylpyrimidin-2-yl)aminocarbonyl]-3-methyl-2-pyridinesulfonamide-1-oxide | HCID 14653190 | — |
反応手順
To a stirring solution of the N-oxide of 3-methyl-2-pyridinesulfonamide (150 mg, 0.79 mmol) and the phenylcarbamate of 4,6-dimethyl-2-aminopyrimidine (194 mg, 0.79 mmol) in 3 mL of CH3CN was added DBU (121 mg, 0.79 mmol). The solution was stirred for 15 minutes. Three mL of H2O, then 3 mL of 5% HCl was added to the reaction and the resulting solid was collected,d m.p. 161°-163° C. NMR (200 MHz, d6 -DMS0) δ 2,36 (s, 6H), 2.59 (s, 3H), 6.97 (s, 1H), 7.4 (d, 1H), 7.5 (d, 1H), 8.3 (d, 1H), 10.6 (br s, 1H) and 13.3 (br s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04900353 |
| 出典データセット | uspto-grants-1990_02 |
| ORD ID | ord-f5f749710f3f412ab04d2b7bc074b7aa |
| 出典メモ | uspto-grants-1990_02 |