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Water → N-(1-methyl-2-pyrrolidylmethyl)-7-methylsulfamoyl-1,4-benzodioxane-5-carboxamide

HRID 127415
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 127415
[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]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

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

Produkt 1

HCID 24834936N-(1-methyl-2-pyrrolidylmethyl)-7-methylsulfamoyl-1,4-benzodioxane-5-carboxamideAusbeute 78,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212Chloroform
Lösungsmittel
2×

Versuchsvorschrift

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%).

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-fa122b0d28404cc7b6502a93ff98d088
Quelldatensatz
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04255580

Notizen zur Reaktion

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