Reacción #8942

ord-02bfd6ae3cc9411485ab357305a1bce2

Disolventes

Condiciones de reacción

Temperatura
0°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroA 100 mL round bottom flask equipped with magnetic stirring bar and N2 inlet
  2. 2
    Concentraciónthen concentrated in vacuo
  3. 3
    Otropartitioned between ethyl acetate and saturated sodium bicarbonate
  4. 4
    LavadoThe combined organics were washed with brine
  5. 5
    Secadodried over Na2SO4
  6. 6
    Concentraciónconcentrated in vacuo
  7. 7
    Otroto yield 3.4 g crude product

Procedimiento

A 100 mL round bottom flask equipped with magnetic stirring bar and N2 inlet was charged with 2.5 g benzyl 3-chlorosulfonyl-2(R)-methylpropionate in 25 mL CH2Cl2. The solution was cooled to 0° C. and charged with 1.57 mL (1.0 eq.) 4-benzylpiperazine and 1.26 mL NEt3. The reaction was stirred for 1 hour then concentrated in vacuo and partitioned between ethyl acetate and saturated sodium bicarbonate. The combined organics were washed with brine, dried over Na2SO4, and concentrated in vacuo to yield 3.4 g crude product. Flash chromatography (80:20 ethyl acetate/hexane) yielded 3.0 g pure product.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07091219B2uspto-grants-2006_08