HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Chloroform → N-(1-allyl-2-pyrrolidylmethyl)-7-methylsulfamoyl-1,4-benzodioxane-5-carboxamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Chloroform | HCID 6212 | — |
| Edukt | 1-(Allyl)pyrrolidine-2-methylamine | HCID 117296 | — |
| Edukt | 7-Methylsulfamoyl-1,4-benzodioxane-5-carbonyl chloride | HCID 20544720 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | N-(1-allyl-2-pyrrolidylmethyl)-7-methylsulfamoyl-1,4-benzodioxane-5-carboxamide | HCID 24834937 | 49% |
Reaktionsschritte
85 g of levorotatory 1-allyl-2-aminomethyl-pyrrolidine, 610 cm3 of chloroform, and gradually, 178 g of 7-methylsulfamoyl-1,4-benzodioxane-5-carbonyl chloride at a temperature of from 5°-10° C. were introduced into a balloon flask provided with an agitator and a thermometer. After agitation of the mixture 1.2 liters of water were added and then chloroform was distilled. The remaining solution was filtered and then the base was precipitated with 70 cm3 of 20% ammonia. The crystals formed were dried off and washed with water. After recrystallization from ethyl acetate, 117 g of levorotatory-N-(1-allyl-2-pyrrolidylmethyl)-7-methylsulfamoyl-1,4-benzodioxane-5-carboxamide was produced (M.P.: 101°-102° C.; yield: 49%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04255580 |
| Quelldatensatz | uspto-grants-1981_03 |
| ORD ID | ord-2e13bbeeda4e4c1591186c2292fd1fa7 |
| Quellennotiz | uspto-grants-1981_03 |