Phosphoric Acid → Desvenlafaxine

HRID 860914

Reaktionsgleichung

Reaktionsgleichung von HRID 860914
[CH3:1][N:2]([CH2:4][CH:5]([C:14]1([OH:20])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1)[C:6]1[CH:7]=[CH:8][C:9]([O:12]C)=[CH:10][CH:11]=1)[CH3:3].[Na].C1(S)C=CC=CC=1.OP(O)(O)=O>O>[CH3:1][N:2]([CH2:4][CH:5]([C:14]1([OH:20])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1)[C:6]1[CH:7]=[CH:8][C:9]([OH:12])=[CH:10][CH:11]=1)[CH3:3]

Komponenten

5

Edukt 3

HCID 1004Phosphoric AcidHCID 5656VenlafaxineHCID 66586497SODIUM THIOPHENOXIDE

Produkt 1

HCID 125017Desvenlafaxine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
160 °C

Versuchsvorschrift

Venlafaxine (5.6 g) and benzenethiol sodium salt (6.9 g) are charged to PEG 400 (25 g). The reaction mixture is heated to 160° C. for 5 hours. Then the temperature is lowered and water is added (60 g). The pH is adjusted to 3.5 with H3PO4. The organic by-products are removed by extraction with heptanes (25 g). The pH of the aqueous layer is then adjusted to 9.5 with aqueous ammonia. The precipitate is collected by suction filtration, re-slurried in water (100 g), isolated by suction filtration and dried in vacuo.

Aufarbeitung

  1. customThe organic by-products are removed by extraction with heptanes (25 g)
  2. filtrationThe precipitate is collected by suction filtration, re-slurried in water (100 g)
  3. customisolated by suction filtration
  4. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-45fafbe0bbc64b9b947cd0b54ba8fe40
Quelldatensatz
uspto-grants-2006_12
Patentnummer
US07154001B2

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