Triphenylphosphine → HCID 54294130, compound

Participants

Reaction Steps

3-(2-Acetylthioethyl)-2-vinyloxycarbonylimino-6-trifluoromethoxybenzothiazoline may be obtained in the following manner: ethyl azodicarboxylate (10.5 cc) is added dropwise to triphenylphosphine (17.6 g) dissolved in tetrahydrofuran (150 cc) at 0° C. Stirring is continued for 30 minutes at this temperature. A solution of thiolacetic acid (4.8 cc) and 3-(2-hydroxyethyl)-2-vinyloxycarbonylimino-6-trifluoromethoxybenzothiazoline (11.7 g) in tetrahydrofuran (75 cc) is then added gradually. The reaction is continued for 1 hour at 0° C. and then 1 hour at a temperature in the region of 20° C. After concentration to dryness under reduced pressure (20 mm Hg; 2.7 kPa), the residue obtained is taken up in methanol (50 cc), then filtered and washed once with methanol (50 cc). 3-(2-Acetylthioethyl)-2-vinyloxycarbonylimino-6-trifluoromethoxybenzothiazoline (10.4 g), m.p. 173° C., is obtained.

Provenance & Evidence