Hydrochloric Acid → 2-Hydroxymethyl-3-hydroxy-6-[1-hydroxy-2-(N-tert-butylbenzylamino)ethyl]pyridine Dihydrochloride

HRID 1632834Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1632834
[OH:1][CH:2]([C:16]1[N:21]=[C:20]2[CH2:22][O:23]C(C3C=CC=CC=3)[O:25][C:19]2=[CH:18][CH:17]=1)[CH2:3][N:4]([CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:5]([CH3:8])([CH3:7])[CH3:6].[ClH:32].Cl.Cl.OCCC1C(O)=CC=C(C(O)CN(CC2C=CC=CC=2)C(C)(C)C)N=1>CO>[ClH:32].[ClH:32].[OH:23][CH2:22][C:20]1[C:19]([OH:25])=[CH:18][CH:17]=[C:16]([CH:2]([OH:1])[CH2:3][N:4]([CH2:9][C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:5]([CH3:8])([CH3:7])[CH3:6])[N:21]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 133401776-[1-Hydroxy-2-(N-tert-butylbenzylamino)ethyl]-2-phenyl-4H-1,3-dioxino[5,4-b]pyridineHCID 704550382-hydroxyethyl-3-hydroxy-6-[1-hydroxy-2-(N-tert-butylbenzylamino)ethyl]pyridine dihydrochloride

Produkt 1

HCID 704547582-Hydroxymethyl-3-hydroxy-6-[1-hydroxy-2-(N-tert-butylbenzylamino)ethyl]pyridine Dihydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A solution of 8.40 g. (0.02 mole) 6-[1-hydroxy-2-(N-tert-butylbenzylamino)ethyl]-2-phenyl-4H-1,3-dioxino[5,4-b]pyridine in 75 ml. of methanol containing 10 ml. of concentrated hydrochloric acid was stirred at room temperature for 4 hours, then the solvents were evaporated in vacuo to give a solid. Recrystallization from isopropanol/methanol gave 6.30 g. (74%) of 2-hydroxyethyl-3-hydroxy-6-[1-hydroxy-2-(N-tert-butylbenzylamino)ethyl]pyridine dihydrochloride; m.p. 173°-175° C. (dec.)

Aufarbeitung

  1. customthe solvents were evaporated in vacuo
  2. customto give a solid
  3. customRecrystallization from isopropanol/methanol
  4. customgave 6.30 g

Quellen und Nachweise

ORD-Eintrag
ord-5a94e454ca8740b89298b6944671e089
Quelldatensatz
uspto-grants-1984_10
Patentnummer
US04477671

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