Hydrochloric Acid → 6-(Difluoro-phenyl-methyl)-3,3-dimethyl-2,3-dihydro-1H-pyrrolo[3,2-c]pyridine hydrochloride

HRID 1475445Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1475445
C(OC([N:8]1[C:16]2[CH:15]=[C:14]([C:17]([F:25])([F:24])[C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[N:13]=[CH:12][C:11]=2[C:10]([CH3:27])([CH3:26])[CH2:9]1)=O)(C)(C)C.[ClH:28]>CO>[ClH:28].[F:25][C:17]([F:24])([C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1)[C:14]1[N:13]=[CH:12][C:11]2[C:10]([CH3:27])([CH3:26])[CH2:9][NH:8][C:16]=2[CH:15]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 709812456-(Difluoro-phenyl-methyl)-3,3-dimethyl-2,3-dihydro-pyrrolo[3,2-c]pyridine-1-carboxylic acid tert-butyl ester

Produkt 1

HCID 709811026-(Difluoro-phenyl-methyl)-3,3-dimethyl-2,3-dihydro-1H-pyrrolo[3,2-c]pyridine hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
35 °C

Versuchsvorschrift

A mixture of 6-(difluoro-phenyl-methyl)-3,3-dimethyl-2,3-dihydro-pyrrolo[3,2-c]pyridine-1-carboxylic acid tert-butyl ester (6.22 g, 16.6 mmol), methanol (30 mL) and hydrochloric acid (5M, 30 mL) was stirred at 20° C. for 3 h, at 35° C. for 4 h, then left at 20° C. for 14 h. Mixture was evaporated in vacuo and the residue azeotroped with toluene (×3), isopropanol and methanol (×3). Residue was dried in vacuo at 50° C. for 4 h to give the title compound. MS: [M+H]+=275.

Aufarbeitung

  1. waitleft at 20° C. for 14 h
  2. customMixture was evaporated in vacuo
  3. customthe residue azeotroped with toluene (×3), isopropanol and methanol (×3)
  4. customResidue was dried in vacuo at 50° C. for 4 h

Quellen und Nachweise

ORD-Eintrag
ord-50b4a2546dc54c1f9bb6e59fbe81c0c7
Quelldatensatz
uspto-grants-2015_04
Patentnummer
US09018214B2

Notizen zur Reaktion

Wird geladen…