反应详情

温度

140 °C

A run was conducted according to the instant invention employing a 250 ml Fisher-Porter aerosol compatibility bottle equipped with a magnetic stirrer as the reaction vessel. The reactor was charged with 7.6 grams (75 mmols) of lithium acetate dihydrate, 3.1 grams (10 mmols) of silver sulfate, 50 ml of acetic acid, 25 ml of acetic anhydride, and 10.7 grams (198.1 mmols) of butadiene charged from the vapor phase. The reactor was pressured to 30 psig with oxygen, placed in an oil bath and heated to 140° C. About one hour was required to bring the temperature of the bath up to the desired reaction temperature. The reaction was conducted for four hours during which the reactor was pressured intermittently to 120 psig with oxygen and then the reactor was allowed to cool overnight, and the reaction continued the following day for an additional 5 hour reaction period. Again during this period, the reactor was pressured intermittently to 120 psig with oxygen. At the end of the reaction period (total of 9 hours), the reactor was vented and the reaction mixture was filtered, and the filtrate then transferred to a distilling flask. The acetic acid was distilled away under 65 mm mercury pressure. There was also recovered 2.2 grams of unreacted butadiene in a cold trap. The distillation residue was mixed with ether, filtered through diatomaceous earth and the filtrate was washed with water, washed with sodium carbonate solution, then dried over magnesium sulfate and filtered. The ether was distilled away at atmospheric pressure. The reaction residue then weighed 14.8 grams and was analyzed by gas-liquid phase chromatography (GLC). This analysis showed that there had been produced 10.23 grams (59.5 mmols) of 1,2-diacetoxy-3-butene and 2.90 grams (16.9 mmols) of 1,4-diacetoxy-2-butene for a yield of diacetoxybutenes of 39 percent based on butadiene charged.

1. customequipped with a magnetic stirrer as the reaction vessel
2. additioncharged from the vapor phase
3. customplaced in an oil bath
4. customreaction temperature
5. waitThe reaction was conducted for four hours during which
6. temperatureto cool overnight
7. customfor an additional 5 hour
8. customreaction period
9. waitAgain during this period
10. customAt the end of the reaction period (total of 9 hours)
11. filtrationthe reaction mixture was filtered
12. customthe filtrate then transferred to a distilling flask
13. distillationThe acetic acid was distilled away under 65 mm mercury pressure
14. additionThe distillation residue was mixed with ether
15. filtrationfiltered through diatomaceous earth
16. washthe filtrate was washed with water
17. washwashed with sodium carbonate solution
18. dry with materialdried over magnesium sulfate
19. filtrationfiltered
20. distillationThe ether was distilled away at atmospheric pressure