Acetone → SAR-407899 hydrochloride dihydrate

HRID 2370255Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2370255
[ClH:1].[NH:2]1[CH2:7][CH2:6][CH:5]([O:8][C:9]2[CH:10]=[C:11]3[C:16](=[CH:17][CH:18]=2)[C:15](=[O:19])[NH:14][CH:13]=[CH:12]3)[CH2:4][CH2:3]1.CC(C)=[O:22]>O>[OH2:8].[OH2:22].[ClH:1].[NH:2]1[CH2:3][CH2:4][CH:5]([O:8][C:9]2[CH:10]=[C:11]3[C:16](=[CH:17][CH:18]=2)[C:15](=[O:19])[NH:14][CH:13]=[CH:12]3)[CH2:6][CH2:7]1

Komponenten

4

Edukt 2

HCID 180AcetoneHCID 426359186-[(Piperidin-4-yl)oxy]isoquinolin-1(2H)-one--hydrogen chloride (1/1)

Produkt 1

HCID 86675574SAR-407899 hydrochloride dihydrate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
55 °C

Versuchsvorschrift

10 g crude 6-(Piperidin-4-yloxy)-2H-isoquinolin-1-one hydrochloride were dissolved in 25 mL water at 70 C. The solution was cooled to 55° C. and 75 mL acetone were added. The mixture was cooled to room temperature within 3 hours and left standing for two days for crystallization. After cooling (4° C.) for 6 hours the product was isolated via filtration, washed with acetone/water (3:1) and dried in vacuum. 7.9 g (purity 97.1%) of 6-(Piperidin-4-yloxy)-2H-isoquinolin-1-one hydrochloride dihydrate were obtained. Water content (Karl Fischer): 10.52%

Aufarbeitung

  1. temperatureThe mixture was cooled to room temperature within 3 hours
  2. waitleft
  3. customstanding for two days for crystallization
  4. temperatureAfter cooling (4° C.) for 6 hours the product
  5. customwas isolated via filtration
  6. washwashed with acetone/water (3:1)
  7. customdried in vacuum

Quellen und Nachweise

ORD-Eintrag
ord-09224a2d95eb478e920de3b60354b2c8
Quelldatensatz
uspto-grants-2014_04
Patentnummer
US08710078B2

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