Ethylene Glycol → 1-(2-Bromo-10,11-dihydro-dibenzo[b,f]thiepin-10-yl)-piperazine

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Reaction Steps

47.2 g of 1-carbethoxy-4-(2-bromo-10,11-dihydro-dibenzo[b,f]thiepin-10-yl)-piperazine hydrochloride, 585 ml of ethylene glycol, 32.8 g of potassium hydroxide and 1.95 ml of water are heated to 160° C for 90 minutes. Then the mixture is poured on to water and extracted with chloroform. The organic solution is extracted with 2-N hydrochloric acid. The hydrochloric acid solution is made alkaline, extracted with chloroform, washed with water, dried over magnesium sulphate and concentrated under reduced pressure. There is obtained crystalline 1-(2-bromo-10,11-dihydro-dibenzo[b,f]thiepin-10-yl)-piperazine of melting point 112°-115° C.

Provenance & Evidence