1,4-Dioxane → HCID 178441228, Verbindung

HRID 406280Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 406280
CC([N:5]([C@H:9]1[CH2:12][C@H:11]([O:13][C:14]2[CH:19]=[C:18]([F:20])[C:17]([C:21]([CH3:24])([CH3:23])[CH3:22])=[C:16]([F:25])[CH:15]=2)[CH2:10]1)C(=O)[O-])(C)C.O1CCOCC1>Cl>[CH3:24][C:21]([C:17]1[C:16]([F:25])=[CH:15][C:14]([O:13][C@H:11]2[CH2:10][C@H:9]([NH2:5])[CH2:12]2)=[CH:19][C:18]=1[F:20])([CH3:22])[CH3:23]

Komponenten

4

Edukt 2

HCID 312751,4-DioxaneHCID 178441233HCID 178441233, Verbindung

Produkt 1

HCID 178441228HCID 178441228, VerbindungAusbeute 77,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

1,1-dimethylethyl(trans-3-{[4-(1,1-dimethylethyl)-3,5-difluorophenyl]oxy}cyclobutyl)carbamate (257 mg, 0.723 mmol) was stirred in 4M HCl in dioxane (5 mL, 20 mmol) overnight and then concentrated in vacuo and loaded onto an SCX cartridge (10 g) and eluted with MeOH (3 column volumes) and then flushed with ammonia in MeOH. Concentration of the product containing fractions in vacuo gave the title compound (142.3 mg).

Aufarbeitung

  1. concentrationconcentrated in vacuo
  2. washeluted with MeOH (3 column volumes)
  3. customflushed with ammonia in MeOH
  4. additionConcentration of the product containing fractions in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-77cc67c5070c4109934745d28da33a67
Quelldatensatz
uspto-grants-2014_06
Patentnummer
US08754101B2

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