(1S,2S)-2-(Diphenylphosphino)-2,3-dihydro-1H-inden-1-aminiumtetrafluoroborate,min.97% synthesis

Yield:1222630-42-3 72%

Reaction Conditions:

with tetrafluoroboric acid in dichloromethane;water at 20; for 0.5 h;Inert atmosphere;

Steps:

1.1i (1S,2S)-2-(diphenylphosphino)-2,3-dihydro-1H-inden-1-ammonium tetrafluoroborate

To a solution of (1 S,2S)-2-(diphenylphosphino)-2,3-dihydro-1H-inden-1-amine (0.50 g, 1.58 mmol) in CH₂Cl₂ (10 mL) was added an aqueous solution of HBF₄ (0.21 mL, 48 wt %) dropwise via syringe. After stirring for 30 minutes at ambient temperature the organic layer was removed, dried over MgSO₄, and then reduced to dryness leaving a pale yellow solid (1i). The solid was redissolved in CH₂Cl₂ (2 mL) and then hexanes was added to afford a pale yellow solid which was filtered off and dried in vacuo. Yield 0.46 g (72%). ¹H NMR (300 MHz, CD₂Cl₂): d 2.78 (dd, 1H, CHPPh₂, 3.36, 3.48 (m, 2H, CH₂), 4.47 (d, 1H, CHNH₃), 7.10-7.60 (br m, 14H, Ar). ³¹P NMR (121.4 MHz, CD₂Cl₂): d -6.4 (s). ¹⁹F NMR (282.3 MHz, CD₂Cl₂): d -148.0 (s).

References:

US2012/46479,2012,A1 Location in patent:Page/Page column 10