HCID 58124946, compound → HCID 58124797, compound

Participants

Reaction Steps

A solution of 550 mg of 12c in 4 ml of 1M tetra-n-butyl ammonium fluoride in THF was stirred at RT for 1 h. The reaction mixture was diluted with 25 ml of 5% aq. NH4Cl and the product was extracted with ethyl acetate. The organic layer was washed twice with sat. aq. NaCl, dried and concentrated. The crude material was purified by chromatography over silica gel, using a gradient of dichloromethane/ethyl acetate gradient as eluent. This provide 250 mg of 12d as a colorless oil. Rf 0.25 (CH2Cl2-ethyl acetate 8/2); MS-ESI: [M+1] 232.3, NMR (CDCl3) δ 1.32 (s, 6, 2×CH3), 1.48 (s, 9, tertC4H9), 1.55 (m, 2, CH2), 1.88 (m, 2, CH2), 2.88 (s, 3, NCH3), 3.02 (m, 2, CH2).

Provenance & Evidence