1,4-Dioxane hydrochloride → (2R)-N-cyclopropyl-N-{(1R)-1-[1-(3-methoxypropyl)-3-methyl-1H-indazol-6-yl]ethyl}morpholine-2-carboxamide hydrochloride

HRID 922413Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 922413
[CH:1]1([N:4]([C@@H:20]([C:22]2[CH:30]=[C:29]3[C:25]([C:26]([CH3:36])=[N:27][N:28]3[CH2:31][CH2:32][CH2:33][O:34][CH3:35])=[CH:24][CH:23]=2)[CH3:21])[C:5]([C@@H:7]2[O:12][CH2:11][CH2:10][N:9](C(OC(C)(C)C)=O)[CH2:8]2)=[O:6])[CH2:3][CH2:2]1.[ClH:37].O1CCOCC1>C(Cl)(Cl)Cl>[ClH:37].[CH:1]1([N:4]([C@@H:20]([C:22]2[CH:30]=[C:29]3[C:25]([C:26]([CH3:36])=[N:27][N:28]3[CH2:31][CH2:32][CH2:33][O:34][CH3:35])=[CH:24][CH:23]=2)[CH3:21])[C:5]([C@@H:7]2[O:12][CH2:11][CH2:10][NH:9][CH2:8]2)=[O:6])[CH2:3][CH2:2]1

Komponenten

4

Edukt 2

HCID 204431481,4-Dioxane hydrochlorideHCID 68308651HCID 68308651, Verbindung

Produkt 1

HCID 86707855(2R)-N-cyclopropyl-N-{(1R)-1-[1-(3-methoxypropyl)-3-methyl-1H-indazol-6-yl]ethyl}morpholine-2-carboxamide hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

To a solution of tert-butyl (2R)-2-[(cyclopropyl{(1R)-1-[1-(3-methoxypropyl)-3-methyl-1H-indazol-6-yl]ethyl}amino)carbonyl]morpholine-4-carboxylate (44.4 mg) in chloroform (2.0 mL) was added 4-normal hydrogen chloride-dioxane solution (0.75 mL) under ice-cooling, and the mixture was stirred at room temperature for 20 hours. The reaction solution was concentrated under reduced pressure, and the resulting residue was dissolved in water (1 mL), and then washed with diethyl ether. The aqueous layer was freeze-dried to give (2R)-N-cyclopropyl-N-{(1R)-1-[1-(3-methoxypropyl)-3-methyl-1H-indazol-6-yl]ethyl}morpholine-2-carboxamide hydrochloride [Ex(3-1)] (25 mg) as a colorless powder.

Aufarbeitung

  1. temperaturecooling
  2. concentrationThe reaction solution was concentrated under reduced pressure
  3. dissolutionthe resulting residue was dissolved in water (1 mL)
  4. washwashed with diethyl ether
  5. customThe aqueous layer was freeze-dried

Quellen und Nachweise

ORD-Eintrag
ord-417c31e79b1d4b73a77f468eba88e839
Quelldatensatz
uspto-grants-2016_03
Patentnummer
US09278944B2

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