Sulfuric Acid → 1,1'-Oxydi(butan-2-ol)

温度

100 °C

A 500 ml, three neck, round bottom flask equipped with magnetic stirrer, internal thermometer, addition funnel, condenser, argon supply, and heating mantle, is flushed with argon. Then 1,2-butanediol (about 270 g, about 3 moles, Aldrich) is added and sodium metal (about 1.2 g, about 0.05 moles, Aldrich) is added and the sodium is allowed to dissolve. Then the reaction mixture is heated to about 100° C. and epoxybutane (about 71 g. about 1 mole, Aldrich) is added dropwise with stirring. Heating is continued until the reflux of epoxybutane has ceased and heating is continued for an additional hour to drive the conversion to completion. The reaction mixture is neutralized with sulfuric acid, the salts are removed by filtration, and the liquid is fractionally distilled under vacuum to recover the excess butanediol. The desired ether is obtained as a residue. Optionally, it is purified by further vacuum distillation.

1. customA 500 ml, three neck, round bottom flask equipped with magnetic stirrer
2. additioninternal thermometer, addition funnel, condenser, argon supply
3. temperatureheating mantle
4. customis flushed with argon
5. dissolutionto dissolve
6. temperatureHeating
7. temperatureheating
8. waitis continued for an additional hour
9. customthe salts are removed by filtration
10. distillationthe liquid is fractionally distilled under vacuum
11. customto recover the excess butanediol
12. customThe desired ether is obtained as a residue
13. distillationOptionally, it is purified by further vacuum distillation

ORDレコード

ord-1a0b995a8d4b4e899ac17c2196ca5293

出典データセット

uspto-grants-1998_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05747443