Hydrochloric Acid → 2-(Aminomethyl)-3,5-di-tert-butylphenol hydrochloride

HRID 1173301Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1173301
Cl.[Cl:2]CC([NH:6][CH2:7][C:8]1[C:13]([OH:14])=[CH:12][C:11]([C:15]([CH3:18])([CH3:17])[CH3:16])=[CH:10][C:9]=1[C:19]([CH3:22])([CH3:21])[CH3:20])=O>C(O)C>[ClH:2].[NH2:6][CH2:7][C:8]1[C:9]([C:19]([CH3:20])([CH3:21])[CH3:22])=[CH:10][C:11]([C:15]([CH3:18])([CH3:17])[CH3:16])=[CH:12][C:13]=1[OH:14]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 687174522-Chloro-N-(2,4-di-tert-butyl-6-hydroxybenzyl)acetamide

Produkt 1

HCID 452597712-(Aminomethyl)-3,5-di-tert-butylphenol hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
85 °C

Versuchsvorschrift

To a solution of 50 mL ethanol and 15 mL conc. hydrochloric acid was added 4.35 g (0.014 mol) of the product of Step A and the reaction mixture was stirred and heated to 85° C. using an external oil bath for 3 h. The reaction mixture was then cooled to room temperature and evaporated in vacuo. Excess water was removed from the product mixture by azeotropic distillation of added portions of toluene on a rotary evaporator. The residue was triturated with ether and dried overnight in vacuo to afford the title compound as a white crystalline solid.

Aufarbeitung

  1. customfor 3 h
  2. temperatureThe reaction mixture was then cooled to room temperature
  3. customevaporated in vacuo
  4. customExcess water was removed from the product mixture by azeotropic distillation of added portions of toluene on a rotary evaporator
  5. customThe residue was triturated with ether
  6. customdried overnight in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-687d2b360f4f4ee79868c9be6a3d7dff
Quelldatensatz
uspto-grants-2010_11
Patentnummer
US07834062B2

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