Hydrochloric Acid → HCID 22326703, Verbindung

HRID 916633Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 916633
C([N:4]1[C:12]2[C:7](=[C:8]([O:13][CH2:14][CH2:15][Cl:16])[CH:9]=[CH:10][CH:11]=2)[CH:6]=[N:5]1)(=O)C.Cl>CO>[Cl:16][CH2:15][CH2:14][O:13][C:8]1[CH:9]=[CH:10][CH:11]=[C:12]2[C:7]=1[CH:6]=[N:5][NH:4]2

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 22350151HCID 22350151, Verbindung

Produkt 1

HCID 22326703HCID 22326703, VerbindungAusbeute 96,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
65 °C

Versuchsvorschrift

A stirred solution of 1-acetyl-4-(2-chloroethoxy)-indazole (1.50 g, 6.3 mmol) in methanol is treated with hydrochloric acid (6.3 ml, 1.0 M HCl in Et2O, 6.3 mmol) at room temperature, heated at 65° C. under nitrogen for 18 hr, cooled to room temperature and concentrated in vacuo. The resultant residue is neutralized with 1 N NaOH (6.0 ml) and diluted with H2O and ethyl acetate. The phases are separated and the aqueous phase is extracted with ethyl acetate. The combined organic phases are washed with water and saturated NaCl, dried over Na2SO4 and concentrated in vacuo to afford the title product (1.2 g) as a yellow solid, identified by NMR and mass spectral analyses.

Aufarbeitung

  1. temperaturecooled to room temperature
  2. concentrationconcentrated in vacuo
  3. additiondiluted with H2O and ethyl acetate
  4. customThe phases are separated
  5. extractionthe aqueous phase is extracted with ethyl acetate
  6. washThe combined organic phases are washed with water and saturated NaCl
  7. dry with materialdried over Na2SO4
  8. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-b3c126df56ce49b0a2428b32c8fefff9
Quelldatensatz
uspto-grants-2007_09
Patentnummer
US07271180B2

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