Ether hydrochloride → cis-3-[(4-propoxy-1H-indazol-5-yl)oxy]cyclohexanamine hydrochloride

HRID 1269937Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1269937
[ClH:1].C(OCC)C.[CH2:7]([O:10][C:11]1[C:19]([O:20][C@@H:21]2[CH2:26][CH2:25][CH2:24][C@H:23]([NH2:27])[CH2:22]2)=[CH:18][CH:17]=[C:16]2[C:12]=1[CH:13]=[N:14][NH:15]2)[CH2:8][CH3:9]>CO>[ClH:1].[CH2:7]([O:10][C:11]1[C:19]([O:20][C@@H:21]2[CH2:26][CH2:25][CH2:24][C@H:23]([NH2:27])[CH2:22]2)=[CH:18][CH:17]=[C:16]2[C:12]=1[CH:13]=[N:14][NH:15]2)[CH2:8][CH3:9]

Komponenten

4

Edukt 2

HCID 10953452Ether hydrochlorideHCID 69432506cis-3-[(4-propoxy-1H-indazol-5-yl)oxy]cyclohexanamine

Produkt 1

HCID 69433087cis-3-[(4-propoxy-1H-indazol-5-yl)oxy]cyclohexanamine hydrochlorideAusbeute 83 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

Under a nitrogen atmosphere, 1M-hydrochloric acid-diethyl ether (341 μl, 0.341 mmol) was added dropwise to a solution of cis-3-[(4-propoxy-1H-indazol-5-yl)oxy]cyclohexanamine (82.3 mg, 0.284 mmol) in methanol (2 ml) at room temperature. After 1 hour, the mixture thus obtained was concentrated under reduced pressure and the resulting residue was crystallized from ethyl acetate, followed by filtration under reduced pressure, and then drying. The solid thus obtained was washed with hexane by repulping to obtain cis-3-[(4-propoxy-1H-indazol-5-yl)oxy]cyclohexanamine hydrochloride (76.8 mg, 83%).

Aufarbeitung

  1. customthe mixture thus obtained
  2. concentrationwas concentrated under reduced pressure
  3. customthe resulting residue was crystallized from ethyl acetate
  4. filtrationfollowed by filtration under reduced pressure
  5. customdrying
  6. customThe solid thus obtained
  7. washwas washed with hexane

Quellen und Nachweise

ORD-Eintrag
ord-8d7aa124532f48b88a2e8567996019fe
Quelldatensatz
uspto-grants-2007_04
Patentnummer
US07199147B2

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