Reaction #94598

ord-fe01ba9c7d884a63b445b6e999ea679e

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Temperatureis heated at 130° to 140° C. for 2 hours
  2. 2
    TemperatureAfter cooling
  3. 3
    Washis washed with water
  4. 4
    OtherThe mixture is dried
  5. 5
    Otherevaporated
  6. 6
    Otherto remove solvent
  7. 7
    workup.ADDITION30 ml of ethanol are added to the residue
  8. 8
    Otherobtained
  9. 9
    Othercrystalline precipitates
  10. 10
    Filtrationare collected by filtration

Procedure

A mixture of 3.7 g of α-chloromethyl-2-methoxybenzylalcohol (crude oil) and 10.9 g of 3,4-dimethoxyphenethylamine is heated at 130° to 140° C. for 2 hours. After cooling, chloroform is added to the reaction mixture, and said mixture is washed with water. The mixture is dried and evaporated to remove solvent. 30 ml of ethanol are added to the residue obtained. Then, hydrochloric acid-containing diethylether is added to the ethanol mixture, and crystalline precipitates are collected by filtration. 3.0 g of α-(3,4-dimethoxyphenethylaminomethyl)-2-methoxybenzylalcohol hydrochloride are obtained as crystals. M.p. 142°-143° C.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04131686uspto-grants-1978_12