Sodium Carbonate → HCID 87111012, compound

Participants

Reaction Conditions

Reaction Steps

NBS (13.5 g, 76 mmol) was added to a solution of (3,5-dimethoxyphenyl)bis(3,5-dimethylphenyl)phosphine oxide (30 g, 76 mmol) in CH2Cl2 (400 ml) at 0° C. The resulting suspension was stirred at 0° C. for 1 h. Na2CO3 (saturated, 300 ml) was added to quench the reactions. It was stirred at RT for 30 min and the organic layer was separated. The aqueous layer was extracted with CH2Cl2 (100 ml×2). The combined organic layer washed with water (150 ml×2), brine (200 ml×1) and dried over MgSO4. It was filtered and the solvent was removed to give the crude product as a pale yellow solid (14.3 g) which was sufficiently pure for the next step. The pure product (34.2 g, 93% yield) was obtained by crystallization from ether/Hexane (1/15). 1H NMR (300 MHz, CD2Cl2) δ: 7.32 (br, 2H), 7.28 (br, 2H), 7.21 (br, 2H), 6.67 (d, J=2.7 Hz, 1H), 6.52 (dd, J1=2.7 Hz, J2=14.1 Hz, 1H), 3.90 (s, 3H), 3.69 (s, 3H), 2.34 (s, 12H). 31P NMR (121.5 MHz, CD2Cl2) δ: 31.35.

Provenance & Evidence