Chloroform → N-(1-cyclohexyl-3-pyrrolidyl)-7-methylsulfamoyl-1,4-benzodioxane-5-carboxamide

HRID 127410

반응식

HRID 127410 반응식
[CH:1]1([N:7]2[CH2:11][CH2:10][CH:9]([NH2:12])[CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(Cl)(Cl)Cl.[CH3:17][NH:18][S:19]([C:22]1[CH:23]=[C:24]([C:32](Cl)=[O:33])[C:25]2[O:30][CH2:29][CH2:28][O:27][C:26]=2[CH:31]=1)(=[O:21])=[O:20]>C(O)(=O)C.O>[CH:1]1([N:7]2[CH2:11][CH2:10][CH:9]([NH:12][C:32]([C:24]3[C:25]4[O:30][CH2:29][CH2:28][O:27][C:26]=4[CH:31]=[C:22]([S:19](=[O:21])(=[O:20])[NH:18][CH3:17])[CH:23]=3)=[O:33])[CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

6

반응물 3

HCID 6212ChloroformHCID 36700741-Cyclohexylpyrrolidin-3-amineHCID 205447207-Methylsulfamoyl-1,4-benzodioxane-5-carbonyl chloride

생성물 1

HCID 24834928N-(1-cyclohexyl-3-pyrrolidyl)-7-methylsulfamoyl-1,4-benzodioxane-5-carboxamide수율 61.3%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

84 g of 1-cyclohexyl-3-aminopyrrolidine, 430 ml of chloroform and 146 g of 7-methylsulfamoyl-1,4-benzodioxane-5-carbonyl chloride were introduced into a balloon flask provided with an agitator and a thermometer. After agitation of the mixture, the base was extracted with methylene chloride and then the solvent was evaporated. The crystals formed were dissolved in boiling absolute alcohol and the resulting solution was filtered on carbon black. The crystals produced after cooling were dissolved in a solution of acetic acid in water and then the solution was filtered over carbon black and the base was reprecipitated by the addition of 20% ammonia. 129.5 g of N-(1-cyclohexyl-3-pyrrolidyl)-7-methylsulfamoyl-1,4-benzodioxane-5-carboxamide was produced (M.P.: 160°-161° C.; yield: 61.2%).

후처리

  1. customprovided with an agitator
  2. extractionAfter agitation of the mixture, the base was extracted with methylene chloride
  3. customthe solvent was evaporated
  4. customThe crystals formed
  5. dissolutionwere dissolved
  6. filtrationthe resulting solution was filtered on carbon black
  7. customThe crystals produced
  8. temperatureafter cooling
  9. filtrationthe solution was filtered over carbon black
  10. customthe base was reprecipitated by the addition of 20% ammonia

출처 및 근거

ORD 기록
ord-6254eec193aa4416b8bd8cc4f0848ef1
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04255580

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