Chloroform → N-(1-allyl-2-pyrrolidylmethyl)-7-methylsulfamoyl-1,4-benzodioxane-5-carboxamide

HRID 127413

反応式

HRID 127413 の反応式
[CH2:1]([N:4]1[CH2:8][CH2:7][CH2:6][CH:5]1[CH2:9][NH2:10])[CH:2]=[CH2:3].C(Cl)(Cl)Cl.[CH3:15][NH:16][S:17]([C:20]1[CH:21]=[C:22]([C:30](Cl)=[O:31])[C:23]2[O:28][CH2:27][CH2:26][O:25][C:24]=2[CH:29]=1)(=[O:19])=[O:18]>O>[CH2:1]([N:4]1[CH2:8][CH2:7][CH2:6][CH:5]1[CH2:9][NH:10][C:30]([C:22]1[C:23]2[O:28][CH2:27][CH2:26][O:25][C:24]=2[CH:29]=[C:20]([S:17](=[O:19])(=[O:18])[NH:16][CH3:15])[CH:21]=1)=[O:31])[CH:2]=[CH2:3]

参加物

5

反応物 3

HCID 6212ChloroformHCID 1172961-(Allyl)pyrrolidine-2-methylamineHCID 205447207-Methylsulfamoyl-1,4-benzodioxane-5-carbonyl chloride

生成物 1

HCID 24834937N-(1-allyl-2-pyrrolidylmethyl)-7-methylsulfamoyl-1,4-benzodioxane-5-carboxamide収率 49%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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%).

後処理

  1. customprovided with an agitator
  2. distillationchloroform was distilled
  3. filtrationThe remaining solution was filtered
  4. customthe base was precipitated with 70 cm3 of 20% ammonia
  5. customThe crystals formed
  6. customwere dried off
  7. washwashed with water
  8. customAfter recrystallization from ethyl acetate, 117 g of levorotatory-N-(1-allyl-2-pyrrolidylmethyl)-7-methylsulfamoyl-1,4-benzodioxane-5-carboxamide
  9. customwas produced (M.P.: 101°-102° C.; yield: 49%)

出典と根拠

ORDレコード
ord-2e13bbeeda4e4c1591186c2292fd1fa7
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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