反应详情

3,4,5-Trimethoxyphenyl isocyanate (1.9 g, 9.11 mmol) was added to a solution of 1-(R)-[4-(3,4-dichlorobenzyl)piperidin-1-ylmethyl]-2-methylpropylamine (2.5 g, 7.59 mmol) in methylene chloride (25 ml) under argon atmosphere. The solution was stirred for 45 min., at room temperature, followed by 30 min., at 38° C. The reaction mixture was concentrated in vacuo. The crude product was chromatographed on a silica gel column, eluting with 1.5-2.5% MeOH/CH2Cl2 containing 1% NH4OH to give 1-{1-(R)-[4-(3,4-dichlorobenzyl)piperidin-1-ylmethyl]-2-methylpropyl}-3-(3,4,5-trimethoxyphenyl)urea (3.7 g).

1. waitfollowed by 30 min., at 38° C
2. concentrationThe reaction mixture was concentrated in vacuo
3. customThe crude product was chromatographed on a silica gel column
4. washeluting with 1.5-2.5% MeOH/CH2Cl2 containing 1% NH4OH