Hydrochloric Acid → 8-bromo-7-(4-fluorobenzyl)-1-(3-hydroxypropyl)-3-methyl-1H-purine-2,6(3H,7H)-dione

HRID 2200623Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2200623
[Br:1][C:2]1[N:10]([CH2:11][C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[C:9]2[C:8](=[O:19])[N:7]([CH2:20][CH2:21][CH2:22][O:23]C3CCCCO3)[C:6](=[O:30])[N:5]([CH3:31])[C:4]=2[N:3]=1.Cl>C(O)C>[Br:1][C:2]1[N:10]([CH2:11][C:12]2[CH:13]=[CH:14][C:15]([F:18])=[CH:16][CH:17]=2)[C:9]2[C:8](=[O:19])[N:7]([CH2:20][CH2:21][CH2:22][OH:23])[C:6](=[O:30])[N:5]([CH3:31])[C:4]=2[N:3]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 904026708-bromo-7-(4-fluorobenzyl)-3-methyl-1-(3-(tetrahydro-2H-pyran-2-yloxy)propyl)-1H-purine-2,6(3H,7H)-dione

Produkt 1

HCID 904026238-bromo-7-(4-fluorobenzyl)-1-(3-hydroxypropyl)-3-methyl-1H-purine-2,6(3H,7H)-dioneAusbeute 83,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To a solution of 8-bromo-7-(4-fluorobenzyl)-3-methyl-1-(3-(tetrahydro-2H-pyran-2-yloxy)propyl)-1H-purine-2,6(3H,7H)-dione (26 g, 52.5 mmol) in ethanol (500 mL) was added concentrated HCl (50 mL) and the mixture was stirred at room temperature for 1 h. The mixture was concentrated to half its volume and the product precipitated. The solids were collected and washed with water and ethanol; then dried under vacuum to give 8-bromo-7-(4-fluorobenzyl)-1-(3-hydroxypropyl)-3-methyl-1H-purine-2,6(3H,7H)-dione (18.1 g, 83.9% yield) as white solid. LCMS retention time 1.243 min; LCMS MH+ 411.

Aufarbeitung

  1. concentrationThe mixture was concentrated to half its volume
  2. customthe product precipitated
  3. customThe solids were collected
  4. washwashed with water and ethanol
  5. customthen dried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-3a5c6da931b1425c97ee868723587f04
Quelldatensatz
uspto-grants-2016_06
Patentnummer
US09359359B2

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