反应详情

A 250 mL three-neck flask equipped with a magnetic stirrer, a thermometer and an addition funnel was charged with 25.4 g (200 mmoles) of oxalyl chloride and 75 mL of methyl t-butyl ether (MTBE). Then to the resulting solution was added 20.6 g (100 mmoles) of 93% 3-t-butylperoxy-1,3-dimethylbutanol over a period of 30 minutes at 22°-28° C. The addition funnel was then replaced with a nitrogen gas tube and dry nitrogen gas was slowly bubbled through the reaction mass in order to remove HCl over a period of 4 hours at 25°-30° C. The MTBE, excess oxalyl chloride, and any remaining gas were removed in vacuo using a water aspirator. Obtained was 28.3 g (101% of theory, uncorrected) of a yellow liquid. An IR spectrum ofthe product showed no OH bands and showed carbonyl bands at 1800 cm-1 and 1760 cm-1. The assay of I-2, based upon hydrolyzable chloride content (theory, 12.63%; found, 12.37%), was 97.9% and the corrected yieldwas 98.6%.

1. customA 250 mL three-neck flask equipped with a magnetic stirrer
2. customThe addition funnel was then replaced with a nitrogen gas tube
3. customdry nitrogen gas was slowly bubbled through the reaction mass in order
4. customto remove HCl over a period of 4 hours at 25°-30° C
5. customThe MTBE, excess oxalyl chloride, and any remaining gas were removed in vacuo
6. customObtained