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Hydrochloric Acid → HCID 178485275, Verbindung

HRID 922721
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 922721
C1(C)C=CC=CC=1.C1COCC1.Cl.[OH:14][C@@:15]([C:43]1[CH:44]=[C:45]2[C:50](=[CH:51][CH:52]=1)[CH:49]=[C:48]([C:53]([NH:55][CH3:56])=[O:54])[CH:47]=[CH:46]2)([C:19]1[N:20]=[CH:21][N:22](C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[CH:23]=1)[CH2:16][CH2:17][OH:18]>O.CO>[OH:14][C@@:15]([C:43]1[CH:44]=[C:45]2[C:50](=[CH:51][CH:52]=1)[CH:49]=[C:48]([C:53]([NH:55][CH3:56])=[O:54])[CH:47]=[CH:46]2)([C:19]1[N:20]=[CH:21][NH:22][CH:23]=1)[CH2:16][CH2:17][OH:18]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 1140TolueneHCID 8028TetrahydrofuranHCID 574658086-[(1S)-1,3-Dihydroxy-1-[1-(triphenylmethyl)-1H-imidazol-4-yl]propyl]-N-methyl-2-naphthalenecarboxamide

Produkt 1

HCID 178485275HCID 178485275, VerbindungAusbeute 89 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittel
HCID 962WaterLösungsmittel2×

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

To a mixture of toluene (100 mL), THF (20 mL) and 1 mol/L hydrochloric acid (100 mL) was added 6-[(1S)-1,3-dihydroxy-1-(1-trityl-1H-imidazol-4-yl)propyl]-N-methyl-2-naphthamide (10.0 g, 17.6 mmol). The reaction mixture was stirred vigorously at 60° C. for 2 hr. The reaction mixture was allowed to cool to room temperature. The aqueous layer was separated, and the obtained aqueous layer was washed twice with methyl tert-butyl ether (100 mL and 50 mL). To the obtained aqueous layer was added methanol (10 mL), and then carbonate (10.6 g) and water (10 mL) were added thereto. The obtained slurry was stirred overnight at room temperature. The obtained crystals were collected by filtration, and washed with 10% aqueous methanol. The obtained wet crystals were dried under reduced pressure to give crude crystals (5.56 g). To a mixture of methanol (30 mL) and water (3 mL) were added the crude crystals (4 g). After stirring at 50° C. for 1 hr, water (50 mL) was added to the slurry at 50° C. over 1 hr. The slurry was stirred at 50° C. for 1 hr, and then allowed to cool to room temperature. After stirring for 3 hr at room temperature, the crystals were collected by filtration and washed with water. The obtained wet crystals were dried under reduced pressure to give 6-[(1S)-1,3-dihydroxy-1-(1H-imidazol-4-yl)propyl]-N-methyl-2-naphthamide (3.69 g, 11.3 mmol). yield 89%.

Aufarbeitung

  1. temperatureto cool to room temperature
  2. customThe aqueous layer was separated
  3. washthe obtained aqueous layer was washed twice with methyl tert-butyl ether (100 mL and 50 mL)
  4. additionTo the obtained aqueous layer was added methanol (10 mL)
  5. additioncarbonate (10.6 g) and water (10 mL) were added
  6. stirringThe obtained slurry was stirred overnight at room temperature
  7. filtrationThe obtained crystals were collected by filtration
  8. washwashed with 10% aqueous methanol
  9. customThe obtained wet crystals were dried under reduced pressure
  10. customto give crude crystals (5.56 g)
  11. stirringAfter stirring at 50° C. for 1 hr
  12. stirringThe slurry was stirred at 50° C. for 1 hr
  13. temperatureto cool to room temperature
  14. stirringAfter stirring for 3 hr at room temperature
  15. filtrationthe crystals were collected by filtration
  16. washwashed with water
  17. customThe obtained wet crystals were dried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-462c82395c2243d8a897efa21aefaca3
Quelldatensatz
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09278938B2

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