HCID 86669982, compound → HCID 67150294, compound

Participants

Reaction Steps

A solution of 6 (49.3 mg, 0.11 mmol) in H2O/MeOH/Et3N (7:3:1, 11 mL) was stirred for 16 h at room temperature. The reaction was evaporated to dryness and the residual white powder was purified by Purification Method 1 (100% 0.05 M TEAB) to afford the triethylammonium salt of 7 as a colorless foam (30 mg, 99%): Rf 0.2 (iPrOH/H2O/aq. NH4OH 6:3:1); δH (400 MHz, D2O) 3.82-3.70 (m, 3H, H-3, H-6, H-7), 3.59 (dd, 1H, J1,2 3.4 Hz, J2,3 9.5 Hz, H-4), 3.54-3.43 (m, 3H, H-5, H-8a, H-8b), 2.97 (q, J=7.3 Hz, NCH2CH3, 1.4 equiv.), 1.70-1.20 (m, 4H, H-1a, H-1b, H-2a, H-2b), 1.04 (t, J=7.3 Hz, NCH2CH3, 1.4 equiv.); δC (100 MHz, D2O) 76.2 (d, JC,P 16.3 Hz, C-3), 71.6 (C-7), 69.6, 69.2 (C-5/C-6), 68.3 (C-4), 61.3 (C-8), 46.7 (NCH2CH3), 23.9 (d, JC,P 134.2 Hz, C-1), 18.4 (C-2), 8.3 (NCH2CH3); δP (161.9 MHz, D2O) 24.9. m/z (ESI) 271.0590 [M−H]−, C8H16O8P requires 271.0588.

Provenance & Evidence