Finasteride → Finasteride lithium Bromide

HRID 1839845

Reaktionsgleichung

Reaktionsgleichung von HRID 1839845
[CH3:1][C@@:2]12[C@@H:10]([C:11]([NH:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:9][CH2:8][C@H:7]1[C@@H:6]1[CH2:18][CH2:19][C@H:20]3[NH:26][C:24](=[O:25])[CH:23]=[CH:22][C@:21]3([CH3:27])[C@H:5]1[CH2:4][CH2:3]2.[Br-:28].[Li+:29]>C(Cl)Cl>[CH3:1][C@@:2]12[C@@H:10]([C:11]([NH:13][C:14]([CH3:15])([CH3:16])[CH3:17])=[O:12])[CH2:9][CH2:8][C@H:7]1[C@@H:6]1[CH2:18][CH2:19][C@H:20]3[NH:26][C:24](=[O:25])[CH:23]=[CH:22][C@:21]3([CH3:27])[C@H:5]1[CH2:4][CH2:3]2.[Br-:28].[Li+:29]

Komponenten

4

Edukt 2

HCID 57363FinasterideHCID 82050Lithium Bromide

Produkt 1

HCID 86759320Finasteride lithium Bromide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Into a 100 ml r.b. flask equipped with a magnetic stirrer and a nitrogen inert atmosphere was weighted 3.71 gm of finasteride. Methylene chloride (20 ml) was added and the slurry astirred to dissolve the substrate. To the clear light yellow solution was added 0.87 g of anhydrous lithium bromide. The solid was washed down into the reaction with 5 ml of methylene chloride. The slurry was stirred. Within one minute add 1 drop of n-propanol from a disposable pipette. The slurry was stirred overnight with exclusion of moisture under an inert nitrogen atmosphere. The slurry is filtered on a Buchner funnel and the flask and solid washed with 10 ml of methylene chloride. After drying the solid at 50° C. in vacuum the solid complex weighs 4.17 g. The methylene chloride solution contains 0.35 g of nonvolatile residue.

Aufarbeitung

  1. customflask equipped with a magnetic stirrer
  2. dissolutionto dissolve the substrate
  3. washThe solid was washed down into the reaction with 5 ml of methylene chloride
  4. additionWithin one minute add 1 drop of n-propanol from a disposable pipette
  5. stirringThe slurry was stirred overnight with exclusion of moisture under an inert nitrogen atmosphere
  6. filtrationThe slurry is filtered on a Buchner funnel
  7. washthe flask and solid washed with 10 ml of methylene chloride
  8. customAfter drying the solid at 50° C. in vacuum the solid complex

Quellen und Nachweise

ORD-Eintrag
ord-72e4a8d9898d44bb934a528578204d0f
Quelldatensatz
uspto-grants-2004_01
Patentnummer
US06677453B1

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