反应详情

In 38 ml of ethanol was suspended 10.6 g of methyl 4-(5-acetoxy-2-hydroxybenzyl)-1-piperazinecarbodithioate (compound prepared in Example 6). In a nitrogen atmosphere, 53 ml of conc. hydrochloric acid was added to the suspension at room temperature. After the solid was dissolved, insolubles were removed by filtration, and further the insolubles were washed with 4 ml of ethanol. The filtrate and washing were combined to give a pale brown solution. The solution was stirred for 20 hours at room temperature to give a suspension. The suspension was further stirred at 80° C. for 3 hours, and then stirred for 8 hours at room temperature. The crystalline solid was collected by filtration and washed with ethanol to give 6.34 g of the desired compound as a pale brown crystalline powder, m.p. 200°-202° C. (decomp.).

1. dissolutionAfter the solid was dissolved
2. custominsolubles were removed by filtration
3. washfurther the insolubles were washed with 4 ml of ethanol
4. washThe filtrate and washing
5. customto give a pale brown solution
6. customto give a suspension
7. stirringThe suspension was further stirred at 80° C. for 3 hours
8. stirringstirred for 8 hours at room temperature
9. filtrationThe crystalline solid was collected by filtration
10. washwashed with ethanol