Reacción #950899

ord-3ea2192fe57042aba4126e24d7156033

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe flask was fitted with an additional funnel
  2. 2
    Otrotopped with a drying tube
  3. 3
    workup.ADDITIONwas added dropwise through a dropping funnel to the flask over a period of half an hour
  4. 4
    OtroThe by-product trimethylsilyl chloride was removed in vacuo

Procedimiento

In a nitrogen glove bag 7.27 g (0.05 mole) of N-methyl-N-trimethylsilylacrylamide was placed in a one-necked flask. The flask was fitted with an additional funnel topped with a drying tube. With the flask contents cooled to ice/water temperatures, 9.28 g (0.05 mole) of 4-bromobutyryl chloride was added dropwise through a dropping funnel to the flask over a period of half an hour. The resulting yellow clear mixture was stirred for an additional two hours. The disappearance of the acyl chloride carbonyl band (1800 cm-1) and the increase in intensity of the product amide band (1670 cm-1) was monitored by IR. The by-product trimethylsilyl chloride was removed in vacuo to give 13 g of product. It was used in the next step without further purification.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05560749uspto-grants-1996_10