関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Amino-4,6-dimethoxypyrimidine | HCID 118946 | — |
| 反応物 | 1-[(N-methylsulfonyl-N-methylamino)-sulfonyl]-3-(N-methylsulfonyl-N-methylamino)urea | HCID 23373886 | — |
| 溶媒 | Chlorobenzene | HCID 7964 | — |
| 生成物 | Amidosulfuron | HCID 91777 | 103.2% |
反応手順
32.3 g of 1-[(N-methylsulfonyl-N-methylamino)-sulfonyl]-3-(N-methylsulfonyl-N-methylamino)urea are slurried in 500 ml of chlorobenzene, 15.5 g of 2-amino-4,6-di-methoxypyrimidine are added at 80° C. with stirring, and the mixture is heated for 3 hours at 80° C. After cooling to 20° C., the precipitate is filtered off and washed with 100 ml of chlorobenzene. 36.4 g of the desired product are obtained with a purity of 98.1%, corresponding to a yield of 96.8% of theory. The melting point for the product is 183°-185° C. 5.1 g of N-methylmethanesulfonamide are recovered from the filtrate by distillation, corresponding to a yield of 92.7% of theory.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05414084 |
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| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-06b25bb0346b4fd7a734e7384a16ca50 |
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| 出典メモ | uspto-grants-1995_05 |
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