Hydrochloric Acid → 4-(2,2-Dioxido-3,4,6,7,8,9-hexahydropyrido[2,1-c][1,2,4]thiadiazin-9-yl)phenol

HRID 1748010

Reaktionsgleichung

Reaktionsgleichung von HRID 1748010
[Si]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH:15]2[C:20]3=[N:21][S:22](=[O:26])(=[O:25])[CH2:23][CH2:24][N:19]3[CH2:18][CH2:17][CH2:16]2)=[CH:11][CH:10]=1)(C(C)(C)C)(C)C.Cl>CC(O)=O>[O:26]=[S:22]1(=[O:25])[CH2:23][CH2:24][N:19]2[CH2:18][CH2:17][CH2:16][CH:15]([C:12]3[CH:13]=[CH:14][C:9]([OH:8])=[CH:10][CH:11]=3)[C:20]2=[N:21]1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 667479969-(4-((Tert-butyl(dimethyl)silyl)oxy)phenyl)-3,4,6,7,8,9-hexahydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide

Produkt 1

HCID 667477204-(2,2-Dioxido-3,4,6,7,8,9-hexahydropyrido[2,1-c][1,2,4]thiadiazin-9-yl)phenolAusbeute 101,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

A mixture of 9-(4-((tert-butyldimethylsilyl)oxy)phenyl)-3,4,6,7,8,9-hexahydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide (6.97 g) and 6 M HCl aq. (10.0 mL) in AcOH (100 mL) was stirred at 60° C. for 2 hr. After cooling to room temperature, the solvent was removed in vacuo. The residual solid was recrystallized from MeOH-IPE to give the title compound (5.01 g) as a white solid.

Aufarbeitung

  1. temperatureAfter cooling to room temperature
  2. customthe solvent was removed in vacuo
  3. customThe residual solid was recrystallized from MeOH-IPE

Quellen und Nachweise

ORD-Eintrag
ord-ca85ea92bfdb45f8b09eaefa3d083aee
Quelldatensatz
uspto-grants-2015_10
Patentnummer
US09150591B2

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