1,1'-Carbonyldiimidazole → HCID 20293650, Verbindung

HRID 1660000

Reaktionsgleichung

Reaktionsgleichung von HRID 1660000
[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-42694517cfef4e4fb9bcb4d290aae1b0
Quelldatensatz
uspto-grants-1981_12
Patentnummer
US04306072

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