Reacción #1599343

Ecuación de reacción

1,4-dioxa-spiro[4.5]decane-8-carbaldehyde

malonic acid

piperidine

→

3-(1,4-dioxa-spiro[4.5]dec-8-yl)-acrylic acid

Disolventes

pyridine

Condiciones de reacción

Tratamiento posterior

1. 1
   ConcentraciónAfter 3 h the resulting solution was concentrated
2. 2
   OtroThe residue obtained
3. 3
   Otrowas partitioned between ethyl acetate and water
4. 4
   OtroThe layers were separated
5. 5
   Lavadothe ethyl acetate layer was washed successively with water and brine
6. 6
   SecadoThe ethyl acetate layer was dried over sodium sulfate
7. 7
   Filtraciónwas filtered
8. 8
   Concentraciónconcentrated
9. 9
   Otrodried in vacuo

Procedimiento

A solution of 1,4-dioxa-spiro[4.5]decane-8-carbaldehyde (3.1 g, 18.4 mmol, prepared as in STEP B above), malonic acid (3.8 g, 36.5 mmol), piperidine (0.182 mL, 1.8 mmol) in pyridine (20 mL) was stirred at 70° C. under an argon atmosphere. After 3 h the resulting solution was concentrated. The residue obtained was partitioned between ethyl acetate and water. The layers were separated, and the ethyl acetate layer was washed successively with water and brine. The ethyl acetate layer was dried over sodium sulfate and was filtered, concentrated, and dried in vacuo to yield 3-(1,4-dioxa-spiro[4.5]dec-8-yl)-acrylic acid.

Fuente