Hydrochloric Acid → HCID 67684261, Verbindung

HRID 232762

Reaktionsgleichung

Reaktionsgleichung von HRID 232762
Cl.O1[C:6]2([CH2:11][CH2:10][N:9]([C@H:12]3[CH2:29][C@@:28]4([CH3:30])[C@@H:15]([CH2:16][CH2:17][C@@H:18]5[C@@H:27]4[CH2:26][CH2:25][C@@:23]4([CH3:24])[C@H:19]5[CH2:20][C@H:21]([N:32]5[CH2:36][CH2:35][CH2:34][CH2:33]5)[C@@H:22]4[OH:31])[CH2:14][C@@H:13]3[OH:37])[CH2:8][CH2:7]2)[O:5]CC1.[OH-].[Na+]>O1CCOCC1>[O:5]=[C:6]1[CH2:11][CH2:10][N:9]([C@H:12]2[CH2:29][C@@:28]3([CH3:30])[C@@H:15]([CH2:16][CH2:17][C@@H:18]4[C@@H:27]3[CH2:26][CH2:25][C@@:23]3([CH3:24])[C@H:19]4[CH2:20][C@H:21]([N:32]4[CH2:36][CH2:35][CH2:34][CH2:33]4)[C@@H:22]3[OH:31])[CH2:14][C@@H:13]2[OH:37])[CH2:8][CH2:7]1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 228685452beta-(1,4-Dioxa-8-azaspiro[4.5]dec-8-yl)-16beta-(1-pyrrolidinyl)-5alpha-androstane-3alpha,17beta-diol

Produkt 1

HCID 67684261HCID 67684261, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel2×

Versuchsvorschrift

After adding 42 ml of 10% aqueous hydrochloric acid solution to 5 g of 2β-(1,4-dioxa-8-azaspiro[4.5]dec-8-yl)-16β-(1-pyrrolidinyl)-5α-androstane-3α,17β-diol dissolved in 100 ml of dioxane, the reaction mixture is boiled under reflux for 3 hours. After completion of the reaction, the solution is made alkaline by adding aqueous sodium hydroxide solution, dioxane is distilled off and the residue is diluted with water. After filtering, the precipitate is washed with water until neutral and dried. The crude product is dissolved in acetonitrile, clarified by activated carbon and after filtering off the adsorbent, two thirds of acetonitrile are distilled off. After filtering, the crystalline precipitate is dried to give the title product in a yield of 4.2 g (92.1%), m.p.: 136°-138° C.

Aufarbeitung

  1. temperatureunder reflux for 3 hours
  2. customAfter completion of the reaction
  3. distillationis distilled off
  4. additionthe residue is diluted with water
  5. filtrationAfter filtering
  6. washthe precipitate is washed with water until neutral and
  7. customdried
  8. dissolutionThe crude product is dissolved in acetonitrile
  9. filtrationafter filtering off the adsorbent, two thirds of acetonitrile
  10. distillationare distilled off
  11. filtrationAfter filtering
  12. customthe crystalline precipitate is dried

Quellen und Nachweise

ORD-Eintrag
ord-c48eb3005e4147b0a0f93086501fc686
Quelldatensatz
uspto-grants-1997_01
Patentnummer
US05591735

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