反应详情

To a warm (60° C.) solution of 10.0 g (0.0640 mole) of 4-methyl-o-benzenedithiol, 5.12 g (0.128 mole) of sodium hydroxide in 70 ml of water was added 21.0 g (0.128 mole) of 4-(3-chloropropyl)morpholine. The reaction mixture was stirred at 60° to 65° C. for 30 minutes, cooled and extracted with methylene chloride. After the extract was dried over anhydrous magnesium sulfate and filtered, ethanolic hydrogen chloride was added, and the solvent and excess hydrogen chloride were removed by evaporation in vacuo. The oily residue was crystallized from propanol-2. Recrystallization from methanol-propanol-2 (1.4:1) gave the product, 4,4'-((4-methyl-1,2-phenylene)bis(thio-3,1-propanediyl))bismorpholine dihydrochloride as white crystals, m.p. 233-234° C.

1. temperaturecooled
2. extractionextracted with methylene chloride
3. dry with materialAfter the extract was dried over anhydrous magnesium sulfate
4. filtrationfiltered
5. additionethanolic hydrogen chloride was added
6. customthe solvent and excess hydrogen chloride were removed by evaporation in vacuo
7. customThe oily residue was crystallized from propanol-2
8. customRecrystallization from methanol-propanol-2 (1.4:1)