反应详情

温度

5 °C

The HCl salt of each 2-(2-mercapto-2-methylpropylamino)-1-[2-(2-propynylthio)-2-methylpropyl-amino]benzene fraction was made by separately dissolving the free amine in 100 ml diethyl ether and cooling the mixture in an ice-H2O bath to 5° C. Anhydrous HCl gas was bubbled through the solution for 3 minutes, which resulted in the precipitation of an amorphous beige solid. The HCl gas and diethyl ether were removed by placing the solution in a 40° C. water bath, and passing a nitrogen stream over the solution. The first sample was recrystallized from ethanol and hexane to give 8.5 g (37% yield, 98.5% purity) of a crystalline, white solid. The second fraction required three successive recrystallizations to obtain a similar purity; 6 g (26% yield, 98% purity). A total of 14.5 g (65% yield) of 2-(2-mercapto-2-methylpropylamino)-1-[2-(2-propynylthio)-2-methylpropylamino]benzene hydrochloride was obtained.

1. customAnhydrous HCl gas was bubbled through the solution for 3 minutes
2. customwhich resulted in the precipitation of an amorphous beige solid
3. customThe HCl gas and diethyl ether were removed
4. customin a 40° C.
5. customThe first sample was recrystallized from ethanol and hexane
6. customto give 8.5 g (37% yield, 98.5% purity) of a crystalline, white solid
7. customthree successive recrystallizations
8. customto obtain a similar purity; 6 g (26% yield, 98% purity)