反应详情

A mixture of 1.0 g of 2-(4-methylsulfonylphenylthio)phenylacetic acid and 10 ml of polyphosphoric acid under nitrogen is stirred at 90°-100° C. for 2 hours. The reaction mixture is permitted to cool and then poured into 100 ml of an ice-water slurry. The aqueous solution is basified with 20% sodium hydroxide before being extracted with methylene chloride. The combined extracts are dried and then evaporated to dryness leaving an oil. The oil is chromatographed through a silica gel column with a 2% methanol in methylene chloride eluant. The chromatographed solution is evaporated to dryness providing 10,11-dihydro-2-methylsulfonyl-11-oxodibenzo[b,f]thiepin.

1. temperatureto cool
2. extractionbefore being extracted with methylene chloride
3. customThe combined extracts are dried
4. customevaporated to dryness
5. customleaving an oil
6. customThe oil is chromatographed through a silica gel column with a 2% methanol in methylene chloride eluant
7. customThe chromatographed solution is evaporated to dryness