HCID 131727888, compound → HCID 131727887, compound

Participants

Reaction Steps

A solution of 20 (137 mg, 0.44 mmol) in EtOH (7 mL) containing 10% Pd—C (46 mg) was hydrogenated at 1 atm (1.5 h). The catalyst was filtered and the filtrate was concentrated in vacuo, and then crystallized with isopropyl ether to afford 21 as a solid. Yield, 81%; Rf=0.19 (10% MeOH—CHCl3); mp 108-110° C. (lit.6) mp 106-112° C. for L-isomer); IR (KBr) 3421, 3318, 2871, 1726, 1670, 1514, 1370, 1243, 1160 cm−1; 1H NMR (CD3OD, 300 MHz) δ1.44 (s, 9H), 3.69 (d, J=5.4 Hz, 2H), 4.06 (t, J=5.4 Hz, 1H); 13C NMR (CD3OD, 75 MHz) δ28.7 (3 C), 56.1, 63.2, 80.9, 157.6, 170.1; MS (+CI) 221 [M+1]+; Mr (+CI) 221.113 90 [M+1]+ (calcd for C8H17N2O5, 221.113 74).

Provenance & Evidence