反应详情

The fluoroborate salt of 1-benzyl-2-iminopyrrolidine (6.55 g.; 0.025 mole) is converted to free base (4.36 g.; 0.025 mole -- assuming 100% conversion) by adding 5 ml. of 50% NaOH to an aqueous slurry of the salt and benzene extraction. After drying over K2CO3, the benzene solution is filtered through diatomaceous earth and 3.84 g. (0.025 mole) of m-chlorophenylisocyanate, dissolved in anhydrous benzene, is added. The reaction mixture is stirred at room temperature for 2 hours and then taken to dryness in vacuo to give an oily residue which eventually crystallizes. Recrystallizations from acetonepetroleum ether affords a pure product, 1-(1-benzyl-2 -pyrrolidylidene)-3-(m-chlorophenyl)urea, m.p. = 91°-93° C.

1. additionby adding 5 ml
2. extractionof 50% NaOH to an aqueous slurry of the salt and benzene extraction
3. dry with materialAfter drying over K2CO3
4. filtrationthe benzene solution is filtered through diatomaceous earth and 3.84 g
5. additionis added
6. customto give an oily residue which
7. customeventually crystallizes
8. customRecrystallizations from acetonepetroleum ether