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ChemicalBook CAS DataBase List 4 - boric acid pinacol ester - 9, 9 - dimethyl fluorene
1365692-79-0

4 - boric acid pinacol ester - 9, 9 - dimethyl fluorene synthesis

2synthesis methods
-

Yield:1365692-79-0 90.3%

Reaction Conditions:

with triethylamine;1,3-bis[(diphenylphosphino)propane]dichloronickel(II) in toluene at 80; for 8 h;Inert atmosphere;

Steps:

1.b-3

In a 300-ml three-neck flask, 7.0 g (26.0 mmol) of the compound b-1, 7.57 ml (52.0 mmol) of the compound b-2, 100 ml of toluene, and 20 ml of triethylamine were charged, and 1.4 g of [1, 1 ' -bis (diphenylphosphino) propane] dichloro nickel was added at room temperature in a nitrogenatmosphere under stirring condition. The temperature was increased to 80°C, and stirring was performed for 8 hours. After the reaction, an organic layer was extracted with toluene, was then dried using anhydrous sodium sulfate, and was subsequently refined using a silica gel column (mixture of toluene and heptane: developing solvent), so that 7.45 g of the compound b-3 (white oil) (yield: 90.3%) was obtained.

References:

WO2012/35962,2012,A1 Location in patent:Page/Page column 37; 38

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