反应详情

A solution of triethylamine (2.0 g; 20 mmole) in methylene chloride was added dropwise to a mixture of 1-(3-amino-propyl)-4-(4-chlorobenzyl)piperazine trihydrochloride (7.54 g; 20 mmole) and allyl isocyanate (1.66 g; 20 mmole) in methylene chloride. After the addition was completed the mixture was washed with water and the solvent removed. The resulting orange oil was purified on a silica gel column (methylene chloride/methanol; 9:1), precipitated with ethereal hydrochloric acid, and recrystallized from ethanol/water to provide the title compound (2.1 g; 25% yield) as colorless crystals, m.p. 232°-234° C.

1. additionAfter the addition
2. washwas washed with water
3. customthe solvent removed
4. customThe resulting orange oil was purified on a silica gel column (methylene chloride/methanol; 9:1)
5. customprecipitated with ethereal hydrochloric acid
6. customrecrystallized from ethanol/water