Hydrochloric Acid → HCID 12248299, Verbindung

HRID 1518952Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1518952
[ClH:1].[C:2]([C:6]1[CH:11]=[CH:10][N:9]=[CH:8][CH:7]=1)([CH3:5])([CH3:4])[CH3:3]>>[ClH:1].[C:2]([C:6]1[CH:11]=[CH:10][N:9]=[CH:8][CH:7]=1)([CH3:5])([CH3:4])[CH3:3]

Komponenten

3

Edukt 2

HCID 313Hydrochloric AcidHCID 198784-tert-Butylpyridine

Produkt 1

HCID 12248299HCID 12248299, VerbindungAusbeute 104,7 %

Reaktionsbedingungen

Temperatur
22 °C

Versuchsvorschrift

Add a solution of hydrogen chloride (4M in dioxane, 794.36 mmol, 198.59 mL) to 4-tert-butylpyridine (100 mL, 662 mmol) at 22° C. over 30 minutes. The internal temperature rises to 32° C.; control the exotherm with an ice-water bath and the by adjusting rate of the addition. Stir the mixture at 22° C. for one hour and concentrate. Wash the walls of the flask with EtOH. Dry the resulting solid under vacuum (1 mbar, 23-40° C.) to give the title compound as a white solid (119 g, 99%). MS (m/z): 136 (M-HCl+1).

Aufarbeitung

  1. customrises to 32° C.
  2. customcontrol the exotherm with an ice-water bath and the by adjusting
  3. additionrate of the addition
  4. concentrationconcentrate
  5. washWash the walls of the flask with EtOH
  6. customDry the resulting solid under vacuum (1 mbar, 23-40° C.)

Quellen und Nachweise

ORD-Eintrag
ord-82d522197c6348e1aa34d8143bd5d96d
Quelldatensatz
uspto-grants-2015_07
Patentnummer
US09073856B2

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