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

HRID 127410

反応式

HRID 127410 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-6254eec193aa4416b8bd8cc4f0848ef1
出典データセット
uspto-grants-1981_03
特許番号
US04255580

関連ノート

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