Réaction #1350561

ord-ee09be3eb1c6461d97787fa65958466c

Équation de réaction

O=C1CCCCC1
cyclohexanone
CC(C)(N)CO
2-amino-2,2-dimethylethanol
CC1(C)COC2(CCCCC2)N1
yellow liquid
Rendement 81.4%
CC1(C)COC2(CCCCC2)N1
3,3-Dimethyl-1-oxa-4-azaspiro[4.5]decane
Rendement 81.4%

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    TempératureThe reaction mixture is then heated
  2. 2
    Températureto reflux
  3. 3
    Autrethe by-product water is collected by a Dean-Stark trap
  4. 4
    TempératureAfter 16 hours of heating
  5. 5
    Températureat reflux
  6. 6
    Concentrationis then concentrated under vacuum

Mode opératoire

Into a solution of 45 g (460 mmol) of cyclohexanone in 300 mL of toluene is added 35.6 g (400 mmol) of 2-amino-2,2-dimethylethanol. The reaction mixture is then heated to reflux and the by-product water is collected by a Dean-Stark trap. After 16 hours of heating at reflux, the reaction mixture is allowed to cool to ambient temperature and is then concentrated under vacuum to give 55 g of a yellow liquid. The product, identified by mass spectroscopy (m/z=169) is obtained in an 81.4% yield. The structure is confirmed by 1Hnmr.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US06540795B2uspto-grants-2003_04