1,3,5-Trithiane → 2-{1-(4-Phenoxyphenyl)-1-hydroxyethan-1-yl}-1,3,5-trithiane

温度

-60 °C

In 30 ml of anhydrous tetrahydrofuran was suspended 2.6 g of 1,3,5-trithiane, and 12 ml of 1.6M n-butyl lithium was added dropwise under an argon atmosphere at a temperature of about -20° C. After completion of the dropwise addition, the resulting mixture was stirred for 2 hours. Next, the reaction mixture was cooled to about -60° C., and then a solution of 4.0 g of 4-phenoxyacetophenone dissolved in 10 ml of tetrahydrofuran was dropped thereinto. After completion of the dropping, the reaction temperature was slowly raised to 0° C. The mixture thus obtained was stirred at 0° C. for another 1 hour. Thereafter, the same treatment as in Example 1 was carried out to obtain a crude product, which was then purified by a silica gel column chromatography (chloroform) to give 3.4 g of the desired compound.

1. additionwas added dropwise under an argon atmosphere at a temperature of about -20° C
2. additionAfter completion of the dropwise addition
3. additionwas dropped
4. temperatureAfter completion of the dropping, the reaction temperature was slowly raised to 0° C
5. customThe mixture thus obtained
6. stirringwas stirred at 0° C. for another 1 hour
7. customto obtain a crude product, which
8. customwas then purified by a silica gel column chromatography (chloroform)

ORDレコード

ord-16ba98998bca43b5b108e5d9646c706c

出典データセット

uspto-grants-1991_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05045562