反应详情

15.8 g. (0.1 mol) of 2-oxo-4,5,5-trimethyl-3-thiazoline-oxime and 15.2 g. (0.15 mol) of triethylamine were dissolved in 100 ml. of anhydrous 1,2-dimethoxy-ethane. 16.1 g. (0.15 mol) of dimethylcarbamoyl chloride were added dropwise. The mixture was refluxed for 3 hours and the solvent was distilled off under vacuum. The residue was dissolved in 100 ml. of dichloromethane and washed with water. After the organic phase was dried over sodium sulfate, the solvent was distilled off. The residue was purified chromatographically on silica gel using ether/dichloromethane (9:1) for the elution to yield 2-oxo-4,5,5-trimethyl-3-thiazoline-O-(dimethylcarbamoyl)-oxime, m.p. 108°-110° C.

1. temperatureThe mixture was refluxed for 3 hours
2. distillationthe solvent was distilled off under vacuum
3. dissolutionThe residue was dissolved in 100 ml
4. washof dichloromethane and washed with water
5. dry with materialAfter the organic phase was dried over sodium sulfate
6. distillationthe solvent was distilled off
7. customThe residue was purified chromatographically on silica gel
8. washfor the elution