Reaction #1257955
Related Literature (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05677025
Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: In 200 ml of N,N-dimethylformamide were dissolved with heating 20 g of 3-hydroxyphthalonitrile and 10.55 g of potassium carbonate, to which 20 g of 1-chloroethyl-trimethylsilane were added dropwise at 30° C. in the atmosphere of argon. Immediately after the addition, the mixture was stirred for 36 hours while maintaining the reaction temperature at 85°-100° C. The reaction vessel was then cooled to room temperature and 200 ml of dilute hydrochloric acid was added. The mixture was extracted with 1 liter of toluene. The organic layer was washed well with water and water was removed with magnesium sulfate. Thereafter, toluene was removed by distillation and the residue was purified with a toluene/silica gel column to obtain 16.9 g (yield: 49.9%) of a compound having the formula (XVIII) below. The compound is in the form of white crystals and has a melting point of 67.5° C. The IR spectrum of the compound is shown in FIG. 4. ##STR40## Immediately after the addition while maintaining the reaction temperature at 85°-100° C The mixture was extracted with 1 liter of toluene The organic layer was washed well with water and water was removed with magnesium sulfate Thereafter, toluene was removed by distillation the residue was purified with a toluene/silica gel column
Source ID: ord-26200d04cbbf4b1495ed701ff2a2acb3