関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Aminomethyl-1-ethylpyrrolidine | HCID 117295 | — |
| 反応物 | Methyl-8-methoxy-7-sulfamoyl-1,4-benzodioxane-5-carboxylate | HCID 20544706 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | N-(1-ethyl-2-pyrrolidyl-methyl)-8-methoxy-7-sulfamoyl-1,4-benzodioxane-5-carboxamide | HCID 20293649 | 73% |
反応手順
150 g of methyl-8-methoxy-7-sulfamoyl-1,4-benzodioxane-5-carboxylate and 750 cm3 of ethylene glycol were introduced into a balloon flask. After dissolution, 127 g of 1-ethyl-2-aminomethylpyrrolidine was added and the mixture was heated at 50° C. The resulting solution was dissolved with 2 liters of water and acidified by means of 120 cm3 of acetic acid. The precipitate formed was dried off, washed with water and then dried. The precipitate was then redissolved in 915 cm3 of hot water. The solution was filtered and then the base was precipitated with ammonia. The precipitate was dried off, washed with water and then dried. 144 g of N-(1-ethyl-2-pyrrolidyl-methyl)-8-methoxy-7-sulfamoyl-1,4-benzodioxane-5-carboxamide was produced (M.P.: 110°-115° C.; yield: 73%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04248885 |
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| 出典データセット | uspto-grants-1981_02 |
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| ORD ID | ord-00ee5519eb0e4358a6861214820e0cf5 |
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| 出典メモ | uspto-grants-1981_02 |
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