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

HRID 127411

反応式

HRID 127411 の反応式
[CH2:1]([N:3]1[CH2:7][CH2:6][CH2:5][CH:4]1[CH2:8][NH2:9])[CH3:2].C(Cl)(Cl)Cl.[CH3:14][NH:15][S:16]([C:19]1[CH:20]=[C:21]([C:29](Cl)=[O:30])[C:22]2[O:27][CH2:26][CH2:25][O:24][C:23]=2[CH:28]=1)(=[O:18])=[O:17]>C(Cl)(Cl)Cl.O>[CH2:1]([N:3]1[CH2:7][CH2:6][CH2:5][CH:4]1[CH2:8][NH:9][C:29]([C:21]1[C:22]2[O:27][CH2:26][CH2:25][O:24][C:23]=2[CH:28]=[C:19]([S:16](=[O:18])(=[O:17])[NH:15][CH3:14])[CH:20]=1)=[O:30])[CH3:2]

参加物

5

反応物 3

HCID 6212ChloroformHCID 1172952-Aminomethyl-1-ethylpyrrolidineHCID 205447207-Methylsulfamoyl-1,4-benzodioxane-5-carbonyl chloride

生成物 1

HCID 24834932N-(1-ethyl-2-pyrrolidylmethyl)-7-methylsulfamoyl-1,4-benzodioxane-5-carboxamide収率 66.1%

試薬・触媒・溶媒 1

HCID 22418719Chloroform water溶媒

実験手順

82 g of dextrorotatory 1-ethyl-2-aminomethylpyrrolidine, 600 ccm of chloroform and, gradually, at a temperature of from 5°-10° C., 200 g of 7-methylsulfamoyl-1,4-benzodioxane-5-carbonyl chloride were introduced into a balloon flask with an agitator and a thermometer. After the addition of a liter of water chloroform was distilled and then the remaining solution was filtered. The base was precipitated by the addition of 60 cm3 of 20% ammonia. The crystals formed were dried off, washed with water and then dried. 162 g of dextrorotatory N-(1-ethyl-2-pyrrolidylmethyl)-7-methylsulfamoyl-1,4-benzodioxane-5-carboxamide was produced (M.P.: 136°-137° C.; yield: 66%).

後処理

  1. distillationwas distilled
  2. filtrationthe remaining solution was filtered
  3. customThe base was precipitated by the addition of 60 cm3 of 20% ammonia
  4. customThe crystals formed
  5. customwere dried off
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-2d1a43d94109458ca9f11b224a17d81b
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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