Water → HCID 24834936, 화합물

HRID 1413156노트

반응식

HRID 1413156 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 24834936HCID 24834936, 화합물수율 78.5%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-86195d134c864bc18be0f97dc3bf147a
출처 데이터셋
uspto-grants-1981_02
특허 번호
US04248885

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