Reacción #460004

ord-4bada0933290425db5dc75d93656184c

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONan addition
  2. 2
    Otrois made in portions at room temperature
  3. 3
    workup.DISSOLUTIONcompletely dissolving
  4. 4
    Lavadothe ether solution is washed three times with 10% potassium hydroxide solution and three times with saturated sodium chloride solution
  5. 5
    SecadoThe ether solution is subsequently dried over sodium sulphate
  6. 6
    Otrothe ether and the readily volatile constituents (traces of 2-chloroethyl-vinyl ether) are completely removed in vacuo

Procedimiento

64 g of freshly distilled 2-chloroethyl-vinyl ether is placed into a flask; one drop of concentrated hydrochloric acid is added, and thereupon an addition is made in portions at room temperature, with stirring, of 93 g of 4-phenoxy-phenol (duration of addition about 1 hour). During the addition of 4-phenoxy-phenol, the temperature rises to about 32°- 34° C, with the 4-phenoxy-phenol completely dissolving. After two further hours' stirring, the reaction mixture is diluted with 300 ml of diethyl ether; the ether solution is washed three times with 10% potassium hydroxide solution and three times with saturated sodium chloride solution. The ether solution is subsequently dried over sodium sulphate, and the ether and the readily volatile constituents (traces of 2-chloroethyl-vinyl ether) are completely removed in vacuo. There is obtained 1-(2-chloroethoxy)-1-[(4-phenoxy)-phenoxy]-ethane in the form of colorless oil having a refractive index of nD20 = 1.5516 (yield 98%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04092365uspto-grants-1978_05