Reaktion #446759
ord-e3ab7037faa943f087c1cabb13d88545
Reaktionsgleichung
2,2,6,6-tetramethyl-4-piperidinol
acetone
acetone
→
needles
1,4-dihydroxy-2,2,6,6-tetramethyl-piperidine
Reagenzien
Keine
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeSolvent was removed on a rotary evaporator
- 2Sonstigeto give a white crystalline solid (0.1727 g, 99% yield, mp 161-163)
Vorschrift
In a 100 ml flask, a solution of 0.047 M DMD in acetone (21.2 ml, 1 mmol) was added to a cold stirred solution of 2,2,6,6-tetramethyl-4-piperidinol (0.1572 g, 1 mmol) in acetone (10 ml). The reaction mixture was stirred for two hours in an ice bath. Solvent was removed on a rotary evaporator to give a white crystalline solid (0.1727 g, 99% yield, mp 161-163). Sublimation on the Kugelrohr (110-120°, 1×10-4 mmHg) gave white needles (0.170 g). Measured mp was 162-163; reported mp is 155-159 (Lee et al 1975 and Rozantsey et al 1966).