HCID 15541340, compound → HCID 9829510, compound

Participants

Reaction Steps

As described for the preparation of 27, the reaction of 26 (prepared from 357 mg of 25) with ethyl cyclopropanecarbodithioate and triethylamine gave the thioamide which was mixed with saturated NaHCO3 and extracted with CH2Cl2. The extract was dried (MgSO4) and concentrated. Chromatography of the residue on silica gel with 5% MeOH-0.5% NH4OH—CH2Cl2 and crystallization of the product from Et2O—CH2Cl2-heptane gave 74 mg of 28: mp 169–170° C.; 1H NMR [300 MHz, (CD3)2SO] δ 0.84 (m, 2H), 1.01 (m, 2H), 2.12 (s, 7H), 2.93. 3.00 (s, s, 4H), 3.25 (s, 2H), 3.60 (s, 4H), 3.79 (dd, 1H), 3.94 (m, 2H), 4.12 (t, 1H), 4.83 (s, 2H), 4.92 (m, 1H), 6.86 (d, 2H), 7.07 (t, 1H), 7.17 (m, 3H), 7.49 (dd, 1H).

Provenance & Evidence