Reacción #659893

ord-f87d7ae9aaa0481cb8a4d9ee5db5f77a

Ecuación de reacción

CC1(C)C(=O)C(C)(C)C1=O
2,2,4,4-tetramethyl-1,3-cyclobutanedione
CC(C)C(O)C(C)(C)CO
TMPD glycol
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CC(C)C(=O)C(C)(C)C(=O)OCC(C)(C)C(O)C(C)C
product
Rendimiento 96.0%
CC(C)C(=O)C(C)(C)C(=O)OCC(C)(C)C(O)C(C)C
3-Hydroxy-2,2,4-trimethylpentyl 2,2,4-trimethyl-3-oxopentanoate
Rendimiento 96.0%

Disolventes

Condiciones de reacción

Temperatura
120°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroReaction
  2. 2
    Temperaturawas cooled
  3. 3
    LavadoOrganic layer was washed 4 times at 70° C
  4. 4
    OtroToluene removed

Procedimiento

To a 1-liter round bottom flask was charged 2,2,4,4-tetramethyl-1,3-cyclobutanedione (140.2 g, 1.0 moles), TMPD glycol (146.2 g, 1.0 moles) and potassium carbonate (73 g, 0.53 moles). The mixture was heated to 120° C. and held for 4 hours. Reaction was cooled and 200 mL of toluene added. Organic layer was washed 4 times at 70° C. Toluene removed to provide 275 g of product. GC assay of the product was 95.9% (4.6:1 mixture of two major isomers).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US09029451B2uspto-grants-2015_05