Hydrochloric Acid → HCID 54555650, compound

To a mixture comprising sufficiently dried metal magnesium (120 mmol) and 30 ml of tetrahydrofuran (hereinafter referred to as THF), was gradually added a solution of 120 mmol of the 4-allyl-bromobenzene in 200 ml of THF to prepare a Grignard reagent. To this reagent was added dropwise a solution of trimethyl borate (120 mmol) in 100 ml of THF at a temperature not exceeding -65° C., stirred for a whole day and night. Subsequently, the mixture was kept at 0° C., 200 ml of 10% hydrochloric acid was gradually added thereto at the same temperature, and then the reaction mixture was stirred for 30 min. The mixture thus obtained was extracted twice with 500 ml of diethyl ether, the organic layer was washed with a saturated brine solution, and then the solvent was removed under a reduced pressure. The residue was sufficiently washed with 500 ml of heptane and then dried to obtain 4-allylphenyl boric acid (79 mmol).

1. customexceeding -65° C.
2. customwas kept at 0° C.
3. stirringat the same temperature, and then the reaction mixture was stirred for 30 min
4. customThe mixture thus obtained
5. extractionwas extracted twice with 500 ml of diethyl ether
6. washthe organic layer was washed with a saturated brine solution
7. customthe solvent was removed under a reduced pressure
8. washThe residue was sufficiently washed with 500 ml of heptane
9. customdried

ORD record

ord-7b079be9e50d49d38da6f39a4ba25980

Source dataset

uspto-grants-1999_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05879585