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-578e3d4f72d342daa0d34c6b1a83e9f9

出典データセット

uspto-grants-2001_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06323172B1