反应详情

Prepared analogously to Example 3 by reaction of 11.6 g (0.043 mol) of 2-trifluoromethyl-4-bromoacetyl-thiazole with 23 g (0.086 mol) of N-(2-hydroxyethyl)-2-(4-carbomethoxymethoxyphenyl)-1-methylethylamine. To complete the reaction the mixture is heated to boiling for 6 hours. It is then concentrated in vacuo, and the resulting residue is dissolved in 85 ml of trifluoroacetic acid and, at room temperature, 7 g (0.06 mol) of triethylsilane are added. After 90 hours the solution is poured onto ice, and concentrated ammonia is added, and the mixture is extracted several times with methylene chloride. The organic phase is dried over sodium sulphate and concentrated, and the residue is purified on a silica gel column using toluene/ethyl acetate=8/2 as eluant.

1. customthe reaction the mixture
2. temperatureis heated
3. concentrationIt is then concentrated in vacuo
4. dissolutionthe resulting residue is dissolved in 85 ml of trifluoroacetic acid and, at room temperature
5. additionis added
6. extractionthe mixture is extracted several times with methylene chloride
7. dry with materialThe organic phase is dried over sodium sulphate
8. concentrationconcentrated
9. customthe residue is purified on a silica gel column