Water → 3-(3,7-Dimethyloctyloxy)bromobenzene

温度

70 °C

Under an inert atmosphere, 90 g of 3-bromophenol was dissolved in 600 ml of ethanol. Further, 39 g potassium hydroxide was added to this and the mixture was heated up to 70° C. for dissolution thereof. From a dropping funnel, 126 g of 3,7-dimethylbromooctane was dropped over 15 minutes. After completion of dropping, the mixture was heated to 84° C. and stirred for about 22 hours under heat. After completion of heating, the mixture was left to cool to room temperature. The reaction solution was bisected, 500 ml of water was added to respective portions, then, ethanol was distilled off by an evaporator. The solutions after distilling off of ethanol were combined and trisected, 300 ml of ethyl acetate was added to respective portions to cause liquid separation, and the organic layers were washed with 200 ml of water twice. The organic layers were combined and the solvent was distilled off by an evaporator, then, the residue was dried by heating at 90° C. for 5 hours under vacuum by a rotary pump. About 150 g of 3-(3,7-dimethyloctyloxy)-bromobenzene was obtained as an oily product.

1. temperaturethe mixture was heated to 84° C.
2. temperatureunder heat
3. temperatureAfter completion of heating
4. waitthe mixture was left
5. temperatureto cool to room temperature
6. distillationethanol was distilled off by an evaporator
7. distillationThe solutions after distilling off of ethanol
8. addition300 ml of ethyl acetate was added to respective portions
9. customliquid separation
10. washthe organic layers were washed with 200 ml of water twice
11. distillationthe solvent was distilled off by an evaporator
12. customthe residue was dried
13. temperatureby heating at 90° C. for 5 hours under vacuum by a rotary pump

ORDレコード

ord-47f7d629a9fe45f69ea8c7869ad0ada3

出典データセット

uspto-grants-2011_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08017721B2