Hydrogen Bromide → 1,3-Bis(3,5-dibromophenyl)adamantane

温度

0 °C

After the air inside a 1 litter flask equipped with a thermometer and stirrer was replaced by nitrogen, 43 g of 1,3-dibromoadamantane and 10 g of anhydrous aluminum bromide were placed therein, and then the inside of the flask was cooled to 0° C. Thereto was added 190 g of 1,3-dibromobenzene that was cooled to 5° C. in advance, and the resulting material was agitated and reacted at an inside temperature of 0 to 10° C. for 7 hours. The reaction was carried out while the hydrogen bromide gas that was generated during the reaction was absorbed into an aqueous alkaline solution for the removal of its toxicity. After the completion of the reaction, 130 g of 4% by weight hydrochloric acid was slowly dropped and then the solution was stirred until the orange color of the reaction solution faded away. The agitation was stopped and the resulting solution was allowed to stand and then separated by funnel. The resulting organic phase was washed with water three times. 190 grams of toluene was added to the organic phase after the washing, which was then warmed to remove water under reflux. Then, the organic solution was cooled and the crystal deposited was collected by filtration. The resulting crystal was subjected to washing with toluene, methanol and water, followed by drying under reduced pressure to obtain 44 g of 1,3-bis(3,5-dibromophenyl)adamantane.

1. customAfter the air inside a 1 litter flask equipped with a thermometer and stirrer
2. temperaturewas cooled to 5° C. in advance
3. customreacted at an inside temperature of 0 to 10° C. for 7 hours
4. customwas absorbed into an aqueous alkaline solution for the removal of its toxicity
5. customAfter the completion of the reaction, 130 g of 4% by weight hydrochloric acid
6. additionwas slowly dropped
7. stirringthe solution was stirred until the orange color of the reaction solution
8. customseparated by funnel
9. washThe resulting organic phase was washed with water three times
10. addition190 grams of toluene was added to the organic phase after the washing, which
11. temperaturewas then warmed
12. customto remove water
13. temperatureunder reflux
14. temperatureThen, the organic solution was cooled
15. filtrationthe crystal deposited was collected by filtration
16. washto washing with toluene, methanol and water
17. customby drying under reduced pressure

ORDレコード

ord-056f03b2844a43409ccd9457a545328f

出典データセット

uspto-grants-2006_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07084287B2