反应详情

One drop of dimethylformamide and 1.34 g (10.5 mmol) oxalyl chloride was added to a solution of 3.30 g (8.77 mmol) 2 in 40 ml dichloromethane. After 30 minutes excess oxalyl chloride was removed in a stream of nitrogen. Subsequently a mixture of 0.97 g (21.1 mmol) ethanol and 2.13 g (21.1 mmol) triethylamine was added dropwise at 0° C. It was allowed to reach room temperature and it was stirred for a further 30 minutes. After adding 60 ml water it was extracted with methylene chloride, washed with 0.5 N HCl and water, dried over sodium sulfate and the solvent was removed. Yield 3.38 g (95%) colourless oil.

1. customAfter 30 minutes excess oxalyl chloride was removed in a stream of nitrogen
2. additionwas added dropwise at 0° C
3. customto reach room temperature
4. extractionwas extracted with methylene chloride
5. washwashed with 0.5 N HCl and water
6. dry with materialdried over sodium sulfate
7. customthe solvent was removed