Water → HCID 24834936、化合物

HRID 1413156

反応式

HRID 1413156 の反応式
[CH3:1][N:2]1[CH2:6][CH2:5][CH2:4][CH:3]1[CH2:7][NH2:8].[CH3:9][NH:10][S:11]([C:14]1[CH:15]=[C:16]([C:24](Cl)=[O:25])[C:17]2[O:22][CH2:21][CH2:20][O:19][C:18]=2[CH:23]=1)(=[O:13])=[O:12].O>C(Cl)(Cl)Cl>[CH3:1][N:2]1[CH2:6][CH2:5][CH2:4][CH:3]1[CH2:7][NH:8][C:24]([C:16]1[C:17]2[O:22][CH2:21][CH2:20][O:19][C:18]=2[CH:23]=[C:14]([S:11](=[O:13])(=[O:12])[NH:10][CH3:9])[CH:15]=1)=[O:25]

参加物

5

反応物 3

HCID 962WaterHCID 1173001-Methylpyrrolidine-2-methylamineHCID 205447207-Methylsulfamoyl-1,4-benzodioxane-5-carbonyl chloride

生成物 1

HCID 24834936HCID 24834936、化合物収率 78.5%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

61 g of dextrorotatory 1-methyl-2-aminomethylpyrrolidine, 465 ccm of chloroform and, in portions, 155 g of 7-methylsulfamoyl-1,4-benzodioxane-5-carbonyl chloride, with the temperature being maintained at 5°-10° C., were introduced into a balloon flask provided with an agitator and a thermometer. After agitation of the mixture and the addition of 1,850 cm3 of water, chloroform was distilled and the remaining solution was filtered. The base was precipitated by the addition of 65 cm3 of 20% ammonia. The crystals formed were dried off, washed and dried. 154 g of dextrorotatory-N-(1-methyl-2-pyrrolidylmethyl)-7-methylsulfamoyl-1,4-benzodioxane-5-carboxamide was produced (M.P.: 187°-188° C.; yield: 78.5%).

後処理

  1. additionwere introduced into a balloon flask
  2. customprovided with an agitator
  3. distillationwas distilled
  4. filtrationthe remaining solution was filtered
  5. customThe base was precipitated by the addition of 65 cm3 of 20% ammonia
  6. customThe crystals formed
  7. customwere dried off
  8. washwashed
  9. customdried

出典と根拠

ORDレコード
ord-86195d134c864bc18be0f97dc3bf147a
出典データセット
uspto-grants-1981_02
特許番号
US04248885

関連ノート

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