1-Methylpyrrolidine-2-methylamine → N-(1-methyl-2-pyrrolidylmethyl)-1,4-benzodioxane-5-carboxamide

HRID 2052626

Reaktionsgleichung

Reaktionsgleichung von HRID 2052626
CO[C:3]([C:5]1[C:14]2[O:13][CH2:12][CH2:11][O:10][C:9]=2[CH:8]=[C:7](S(=O)(=O)NC)[CH:6]=1)=[O:4].[CH3:20][N:21]1[CH2:25][CH2:24][CH2:23][CH:22]1[CH2:26][NH2:27]>C(O)(=O)C.O>[CH3:20][N:21]1[CH2:25][CH2:24][CH2:23][CH:22]1[CH2:26][NH:27][C:3]([C:5]1[C:14]2[O:13][CH2:12][CH2:11][O:10][C:9]=2[CH:8]=[CH:7][CH:6]=1)=[O:4]

Komponenten

5

Edukt 2

HCID 1173001-Methylpyrrolidine-2-methylamineHCID 54343297Methyl-7-methylsulfamoyl-1,4-benzodioxane-5-carboxylate

Produkt 1

HCID 53775438N-(1-methyl-2-pyrrolidylmethyl)-1,4-benzodioxane-5-carboxamideAusbeute 112 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittel2×

Versuchsvorschrift

169 g of methyl-7-methylsulfamoyl-1,4-benzodioxane-5-carboxylate, 53 ml of water and 81 g of 1-methyl-2-aminomethylpyrrolidine were introduced into a balloon flask provided with a reflux condenser. The mixture was heated on a water bath until a test sample was totally soluble in dilute acids. The resulting crystals were dissolved in a solution of 50 ml of acetic acid in 1,250 ml of water and then the solution was filtered over carbon black and the base was reprecipitated by the addition of 100 ml of 20% ml of 20% ammonia. The crystals were dried off, washed with water and dried. 182 g of N-(1-methyl-2-pyrrolidylmethyl)-1,4-benzodioxane-5-carboxamide was produced (M.P.: 189°-190° C.; yield 83.6%).

Aufarbeitung

  1. customprovided with a reflux condenser
  2. temperatureThe mixture was heated on a water bath until a test sample
  3. filtrationthe solution was filtered over carbon black
  4. customthe base was reprecipitated by the addition of 100 ml of 20% ml of 20% ammonia
  5. customThe crystals were dried off
  6. washwashed with water
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-c4426c0ad46c4a8da6fb6c852e4769b7
Quelldatensatz
uspto-grants-1980_01
Patentnummer
US04186135

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