Hydrochloric Acid → 4972-11-6

HRID 2301223Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2301223
[ClH:1].[OH:2][N:3]1[C:8]([CH3:10])([CH3:9])[CH2:7][CH:6]([OH:11])[CH2:5][C:4]1([CH3:13])[CH3:12]>C(O)(C)C>[Cl-:1].[OH:2][NH+:3]1[C:8]([CH3:9])([CH3:10])[CH2:7][CH:6]([OH:11])[CH2:5][C:4]1([CH3:13])[CH3:12]

Komponenten

4

Edukt 2

HCID 313Hydrochloric Acid2×HCID 53951,4-Dihydroxy-2,2,6,6-tetramethylpiperidine

Produkt 1

HCID 668682954972-11-6

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel2×

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

67 mL of isopropanol is cooled to 0° C. and saturated with HCl gas. This solution is added dropwise to a mechanically stirred solution of 50 g (0.29 mol) 1-oxyl-2,2,6,6-tetramethyl-4-hydroxypiperidine in 130 mL of isopropanol, maintaining a reaction temperature of about 20° C. by occasionally cooling with an ice bath. The HCl salt is vacuum filtered and washed with isopropanol, giving a pale yellow solid. 5.0 g of this crude product is recrystallized from 100 mL isopropanol affording 3 g of a white crystalline solid, mp>260° C.

Aufarbeitung

  1. temperatureby occasionally cooling with an ice bath
  2. filtrationfiltered
  3. washwashed with isopropanol
  4. customgiving a pale yellow solid
  5. custom5.0 g of this crude product is recrystallized from 100 mL isopropanol affording 3 g of a white crystalline solid, mp>260° C.

Quellen und Nachweise

ORD-Eintrag
ord-8624c1318bd24d639d8572f75b5ce528
Quelldatensatz
uspto-grants-2002_12
Patentnummer
US06500303B1

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