反应详情

温度

140 °C

Another run was conducted according to the instant invention using the same apparatus as employed in the runs of Example I. In this run, the reactor was charged with 2.5 grams (20 mmol) of molybdenum dioxide (MoO2), 6.5 grams (75 mmol) of lithium bromide, 4.6 grams (22.5 mmol) of 1,4-dibromo-2-butene, 50 ml of acetic acid, 25 ml of acetic anhydride and 10.9 grams (201.8 mmol) of butadiene from the vapor phase. The reactor was pressured to 30 psig with oxygen, placed in an oil bath and heated to 140° C. As in the runs of Example I, the reactor was pressured intermittently with oxygen to 120 psig. The reactor required about 30 minutes to reach the 140° C. reaction temperature after which the reaction was conducted for 4.75 hours. At the end of the reaction period, the reactor was vented and the solid materials separated by filtration. The filtrate was distilled to remove acetic acid. The distillation residue was then mixed with ether and water, and the layers were separated. The aqueous layer was extracted with ether, and the combined ether extracts were filtered, washed with water, neutralized with a sodium carbonate solution, and dried over magnesium sulfate. The ether solution was then filtered and the ether removed on a rotary evaporator. There remained 13.5 grams of a dark oil which was analyzed by gas-liquid phase chromatography. The analysis showed that there was obtained 9.3 mmol of 1,2-diacetoxy-3-butene and 31.8 mmol of 1,4-diacetoxy-2-butene for a diacetoxy-butene yield of 20 percent based on the butadiene charged.

1. customplaced in an oil bath
2. customabout 30 minutes
3. customthe 140° C. reaction temperature after which the reaction
4. customAt the end of the reaction period
5. customthe solid materials separated by filtration
6. distillationThe filtrate was distilled
7. customto remove acetic acid
8. additionThe distillation residue was then mixed with ether and water
9. customthe layers were separated
10. extractionThe aqueous layer was extracted with ether
11. filtrationthe combined ether extracts were filtered
12. washwashed with water
13. dry with materialdried over magnesium sulfate
14. filtrationThe ether solution was then filtered
15. customthe ether removed on a rotary evaporator