[C:1]([C:5]1[S:6][C:7]2[CH2:20][CH2:19][C:11]3[N:12]=[C:13]([NH:15]C(=O)C)[S:14][C:10]=3[C:8]=2[N:9]=1)([CH3:4])([CH3:3])[CH3:2].Cl.C(=O)(O)[O-].[Na+]>CCO>[C:1]([C:5]1[S:6][C:7]2[CH2:20][CH2:19][C:11]3[N:12]=[C:13]([NH2:15])[S:14][C:10]=3[C:8]=2[N:9]=1)([CH3:4])([CH3:2])[CH3:3]N-(7-tert-Butyl-4,5-dihydro-benzo[1,2-d;3,4-d′]bisthiazol-2-yl)-acetamide (Stage T.2, 225 mg, 0.732 mmol) was dissolved in EtOH (10 mL), HCl 36% (1.48 g, 14.64 mmol) was then added, and the RM heated to reflux. After 18 hours at reflux the RM was cooled to rt and adjusted to pH 8-9 by the addition of 5% aqueous sodium bicarbonate solution, extracted with EtOAc, and washed two times with H2O. The organic layer was dried over Na2SO4 and evaporated to give the title product (tR 4.408 min (Method F)).
読み込み中…