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Methanesulfonic Acid → Imazosulfuron
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Phenyl chloroformate | HCID 15891 | — |
| 反応物 | 2-Amino-4,6-dimethoxypyrimidine | HCID 118946 | — |
| 反応物 | 2-Chloroimidazo[1,2-a]pyridine-3-sulfonamide | HCID 14422354 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Imazosulfuron | HCID 92433 | 83% |
反応手順
In 30 ml of acetonitrile are dissolved 2.32 g (0.01 mole) of 2-chloroimidazo[1,2-a]pyridine-3-sulfonamide and 2.02 g (0.02 mole) of triethylamine, followed by addition of 1.60 g (0.01 mole) of phenyl chloroformate with stirring at 10° to 20° C. The mixture is further stirred at 20° to 25° C. for 30 minutes, and to the mixture are added 1.00 g (0.010 mole) of methanesulfonic acid and then 1.55 g (0.01 mole) of 2-amino-4,6-dimethoxypyrimidine. The mixture is stirred at 60° C. for 15 minutes. After cooling, the crystals which separates out are collected by filtration and washed with water 3 times with 10 ml of water each. The crystals were then dried in vacuo over P2O5 to give 3.42 g (yield 83.0%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04994571 |
| 出典データセット | uspto-grants-1991_02 |
| ORD ID | ord-f752d89f844e45b0b060b637c77f4630 |
| 出典メモ | uspto-grants-1991_02 |