反应详情

A solution of 3.0 g (31 mmoles) of 4-methyl piperazine and 3.1 g (31 mmoles) of triethyl amine in 40 cc of CH2Cl2 is poured drop by drop in the CH2Cl2 solution containing 7.47 g (25.9 mmoles) of 7-methyl-9-oxo-thioxanthene-3-carbonyl chloride. After approximately 1 hour at room temperature under stirring, the mixture is poured in water, the organic phase is separated and washed again with water. The organic phase is then separated, dehydrated and dried after purification on a flash column (SiO2— eluent: CH2Cl2:AcOEt 9:1) obtaining 4.63 g (50.8%) of a yellow solid, with the following spectral properties:

1. customthe organic phase is separated
2. washwashed again with water
3. customThe organic phase is then separated
4. customdried
5. customafter purification on a flash column (SiO2— eluent: CH2Cl2:AcOEt 9:1)