Water → HCID 24834936、化合物

HRID 127415

反応式

HRID 127415 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-fa122b0d28404cc7b6502a93ff98d088
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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