[CH3:1][O:2][C:3]([C:5]1[S:9][C:8]2[CH:10]=[C:11]([C:14]([O:16][CH2:17][CH:18]=[CH2:19])=[O:15])[CH:12]=[CH:13][C:7]=2[C:6]=1[S:20][CH2:21][C:22]([O:24][CH3:25])=[O:23])=[O:4].[CH2:26]1[CH2:36][CH2:35][N:34]2[C:29](=NCCC2)[CH2:28][CH2:27]1.Br[CH2:38][C:39]([O:41][CH2:42][CH3:43])=[O:40].C([O-])([O-])=O.[K+].[K+].[NH4+].[Cl-]>CN(C=O)C.O>[C:39]([CH2:1][O:2][C:3]1[C:5]2[S:9][C:8]3[CH:10]=[C:11]([NH:34][CH:29]4[CH2:28][CH2:27][CH2:26][CH2:36][CH2:35]4)[CH:12]=[CH:13][C:7]=3[C:6]=2[S:20][C:21]=1[C:22]([OH:24])=[O:23])([OH:41])=[O:40].[CH3:25][O:24][C:22]([C:21]1[S:20][C:6]2[C:7]3[CH:13]=[CH:12][C:11]([C:14]([O:16][CH2:17][CH:18]=[CH2:19])=[O:15])=[CH:10][C:8]=3[S:9][C:5]=2[C:3]=1[O:4][CH2:38][C:39]([O:41][CH2:42][CH3:43])=[O:40])=[O:23]To a solution of 3-methoxycarbonylmethylsulfanyl-benzo[b]thiophene-2,6-dicarboxylic acid 6-allyl ester 2-methyl ester (1.05 g, 2.76 mmol) in DMF was added DBU (0.83 mL, 5.53 mmoL) at room temperature. The resultant mixture was stirred for 24 hours. To this was added ethyl bromoacetate (0.92 mL, 8.28 mmoL) and K2CO3 (1.14 g, 8.26 mmoL). The reaction mixture was stirred for additional 2 hours, then aq. NH4Cl (200 mL and water (300 mL) was added. The white precipate was collected by filtration and washed with water to give the desired compound, 1-ethoxycarbonylmethoxy-3,8-dithia-cyclopenta[a]indene-2,6-dicarboxylic acid 6-allyl ester 2-methyl ester (1.162 g, 97% overall).
Wird geladen…