1,4-Dioxane → HCID 178420570, compound

The zinc chloride solution was charged to the flask by syringe and diluted with 60 ml THF all under a nitrogen atmosphere. The stirrer was started and phenylmagnesium bromide introduced using a dry 20 ml syringe dropwise over 5 min initially forming a precipitate which dissolved by the end of the addition. The reaction mixture was held at 20-25° C. during addition and stirred for a total of 2 hours. The dioxan was then added by syringe causing a fine, white solid to precipitate. The slurry was stirred a further 45 min at 25° C., then filtered via the in-line sintered glass filter. The filter cake was washed with 10 ml THF and blown dry with nitrogen. The filtrate was a pale yellow solution in THF of diphenylzinc (57 mol % Zn, 10.2 mol % Mg). The flask was sealed and stored in a refrigerator.

1. customdropwise over 5 min
2. custominitially forming a precipitate which
3. dissolutiondissolved by the end of the addition
4. additionThe reaction mixture was held at 20-25° C. during addition
5. customto precipitate
6. stirringThe slurry was stirred a further 45 min at 25° C.
7. filtrationfiltered via the in-line sintered glass
8. filtrationfilter
9. washThe filter cake was washed with 10 ml THF
10. customblown dry with nitrogen
11. customThe flask was sealed

ORD record

ord-d9148aa5a4044c5e8dc56df966a758fa

Source dataset

uspto-grants-2001_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06258967B1