Monosodium Citrate → Tofacitinib Citrate

HRID 1775142

Reaktionsgleichung

Reaktionsgleichung von HRID 1775142
[CH3:1][C@H:2]1[C@@H:7]([N:8]([C:10]2[N:18]=[CH:17][N:16]=[C:15]3[C:11]=2[CH:12]=[CH:13][NH:14]3)[CH3:9])[CH2:6][N:5]([C:19]([CH2:21][C:22]#[N:23])=[O:20])[CH2:4][CH2:3]1.Br.[C:25]([O-:37])(=[O:36])[CH2:26][C:27]([CH2:32][C:33]([OH:35])=[O:34])([C:29]([OH:31])=[O:30])[OH:28].[Na+]>O>[CH3:1][C@H:2]1[C@@H:7]([N:8]([C:10]2[N:18]=[CH:17][N:16]=[C:15]3[C:11]=2[CH:12]=[CH:13][NH:14]3)[CH3:9])[CH2:6][N:5]([C:19]([CH2:21][C:22]#[N:23])=[O:20])[CH2:4][CH2:3]1.[CH2:32]([C:27]([OH:28])([C:29]([OH:31])=[O:30])[CH2:26][C:25]([OH:37])=[O:36])[C:33]([OH:35])=[O:34]

Komponenten

4

Edukt 2

HCID 23666341Monosodium CitrateHCID 131734730HCID 131734730, Verbindung

Produkt 1

HCID 10174505Tofacitinib CitrateAusbeute 89,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

Amorphous tofacitinib hydrobromide (0.55 g) was dissolved in water (6 mL). The solution was treated with solid monosodium citrate (0.40 g, 1.69 mmol) and the resulting white suspension was stirred for 16 hours at 25° C. The suspension was filtered, washed with water (2×5 mL) and air-dried for 16 hours at 25° C. to yield 0.63 g of tofacitinib citrate as a white solid.

Aufarbeitung

  1. filtrationThe suspension was filtered
  2. washwashed with water (2×5 mL)
  3. customair-dried for 16 hours at 25° C.

Quellen und Nachweise

ORD-Eintrag
ord-749e280bbddb45d38834f9f5890e8c66
Quelldatensatz
uspto-grants-2016_02
Patentnummer
US09260438B2

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