反应详情

3.040 g of TMHQ, 0.484 g of metallic tin powder and 0.079 g of zinc chloride were suspended in 15 ml of ethyl acetate in an atmosphere of nitrogen. A solution of 7.975 g of phytyl chloride in 10 ml of ethyl acetate was dripped into said suspension over a period of 3 hours under heating and reflux. About 0.1 g metallic tin powder was added eight times, same amount per addition, in order to maintain said tin continuously suspended in the suspension. After addition of the phytyl chloride, the reaction mixture was subjected to heating and reflux for another 3 hours to obtain a reaction mixture of dl-α-tocopherol. The obtained dl-α-tocopherol was acetylated in the same manner as described in Comparative Example 1 without isolating said dl-α-tocopherol to obtain 10.454 of dl-α-tocopheryl acetate. The absorbance of this crude dl-α-tocopheryl acetate was measured: E415 mμ40%EtOH =0.145. Estimation of the crude dl-α-tocopheryl acetate by liquid chromatography indicated that its purity was 76.3% and the yield was 84.5%.

1. customof 3 hours
2. temperatureunder heating
3. temperaturereflux
4. additionper addition
5. temperaturein order to maintain
6. temperatureto heating
7. temperaturereflux for another 3 hours
8. customto obtain
9. customwithout isolating