反应详情

5.0 G. of enriched (-)-(R)-3-{2-[4-(8-fluoro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-yl)-1-piperazinyl]ethyl}-2-oxazolidinone αD20 = -9.5°; α365 = +125.0° (chloroform; c = 2.50%)] are heated under reflux for 18 hours with stirring in 81 ml. of 0.5-M methanesulfonic acid and the mixture is subsequently treated with benzene. The organic phase is washed with water, dried over sodium sulfate and evaporated. The residue is crystallized from n-hexane, and there is obtained racemic 8-fluoro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-ol having a melting point of 89.5°-90° C. The yield is 97%. This compound can be converted in accordance with the procedure described in Example 1 into the 10-chloro compound which can subsequently be used in Example 1 or 11.

1. temperatureunder reflux for 18 hours
2. washThe organic phase is washed with water
3. dry with materialdried over sodium sulfate
4. customevaporated
5. customThe residue is crystallized from n-hexane