Triisopropyl borate → HCID 59439576, compound

Temperature

-78 °C

To a solution of 1,2-diiodo-3,5-dimethylbenzene (0.5 g, 1.40 mmol) in 60 mL in a mixture of THF and Et2O (1:1), was added dropwise at −78° C. isopropylmagnesium chloride (2 M in THF, 0.70 mL, 1.40 mmol). After the mixture was stirred for 2 h at −78° C., B(OiPr)3 (0.96 ml, 4.19 mmol) was added. The solution was warmed to room temperature overnight, then a saturated solution of NH4Cl was added, and the resulting mixture was stirred for 30 min at room temperature. The aqueous layer was extracted with Et2O (50 mL, 3 times), dried over Na2SO4 and concentrated. To the concentrated sample, hexane was added and the resulting precipitate was isolated to provide the products as shown above as non separable mixture.

1. temperatureThe solution was warmed to room temperature overnight
2. stirringthe resulting mixture was stirred for 30 min at room temperature
3. extractionThe aqueous layer was extracted with Et2O (50 mL, 3 times)
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. additionTo the concentrated sample, hexane was added
7. customthe resulting precipitate was isolated
8. customto provide the products

ORD record

ord-0c49cbc2446f409abf8aaea63b9b65cf

Source dataset

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08822720B2