1,1'-Carbonyldiimidazole → HCID 20293650, Verbindung

HRID 127409

Reaktionsgleichung

Reaktionsgleichung von HRID 127409
[CH2:1]([S:3]([C:6]1[CH:7]=[C:8]([C:16]([OH:18])=O)[C:9]2[O:14][CH2:13][CH2:12][O:11][C:10]=2[CH:15]=1)(=[O:5])=[O:4])[CH3:2].C(N1C=CN=C1)(N1C=CN=C1)=O.[CH2:31]([N:33]1[CH2:37][CH2:36][CH2:35][CH:34]1[CH2:38][NH2:39])[CH3:32]>O1CCCC1>[CH2:31]([N:33]1[CH2:37][CH2:36][CH2:35][CH:34]1[CH2:38][NH:39][C:16]([C:8]1[C:9]2[O:14][CH2:13][CH2:12][O:11][C:10]=2[CH:15]=[C:6]([S:3]([CH2:1][CH3:2])(=[O:4])=[O:5])[CH:7]=1)=[O:18])[CH3:32]

Komponenten

5

Edukt 3

HCID 682631,1'-CarbonyldiimidazoleHCID 1172952-Aminomethyl-1-ethylpyrrolidineHCID 205447587-Ethylsulfonyl-1,4-benzodioxane-5-carboxylic acid

Produkt 1

HCID 20293650HCID 20293650, VerbindungAusbeute 76,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

13 g of 7-ethylsulfonyl-1,4-benzodioxane-5-carboxylic acid, 300 ml of tetrahydrofuran and 13 g of carbonyldiimidazole were introduced into a balloon flask provided with an agitator, a thermometer and a condenser. The mixture was agitated at ambient temperature and then 9.5 g of 1-ethyl-2-aminomethylpyrrolidine was added. Agitation was maintained at ambient temperature and then the solvent was evaporated under vacuum. The crystals produced were washed with water and then dried. 14 g of N-(1-ethyl-2-pyrrolidylmethyl)-7-ethylsulfonyl-1,4-benzodioxane-5-carboxamide was produced (M.P.: 118°-119° C.; yield: 73.8%)

Aufarbeitung

  1. customprovided with an agitator
  2. temperatureAgitation was maintained at ambient temperature
  3. customthe solvent was evaporated under vacuum
  4. customThe crystals produced
  5. washwere washed with water
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-9a5a643d93394373bc0f9a3d0e24ae3c
Quelldatensatz
uspto-grants-1981_03
Patentnummer
US04255580

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