Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Methylpyrrolidine-2-methylamine → N-(1-methyl-2-pyrrolidylmethyl)-1,4-benzodioxane-5-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Methylpyrrolidine-2-methylamine | HCID 117300 | — |
| 반응물 | Methyl-7-methylsulfamoyl-1,4-benzodioxane-5-carboxylate | HCID 54343297 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | N-(1-methyl-2-pyrrolidylmethyl)-1,4-benzodioxane-5-carboxamide | HCID 53775438 | 112% |
반응 단계
169 g of methyl-7-methylsulfamoyl-1,4-benzodioxane-5-carboxylate, 53 ml of water and 81 g of 1-methyl-2-aminomethylpyrrolidine were introduced into a balloon flask provided with a reflux condenser. The mixture was heated on a water bath until a test sample was totally soluble in dilute acids. The resulting crystals were dissolved in a solution of 50 ml of acetic acid in 1,250 ml of water and then the solution was filtered over carbon black and the base was reprecipitated by the addition of 100 ml of 20% ammonia. The crystals were dried off, washed with water and dried. 182 g of N-(1-methyl-2-pyrrolidylmethyl)-1,4-benzodioxane-5-carboxamide was produced (M.P.: 189°-190° C.; yield: 83.6%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04255580 |
| 출처 데이터셋 | uspto-grants-1981_03 |
| ORD ID | ord-52d36f660dca4f7a94c7961311a582bd |
| 출처 메모 | uspto-grants-1981_03 |