2-(Methylthio)benzothiazole → Methyl 1,2,3,4-tetrahydro-3-methyl-1-(isobutyl)-2,4-dioxo-6-[2-thioxo-3(2H)-benzothiazolylmethyl]thieno[2,3-d]pyrimidine-5-carboxylate
反応式
Br[CH2:2][C:3]1[S:18][C:6]2[N:7]([CH2:14][CH:15]([CH3:17])[CH3:16])[C:8](=[O:13])[N:9]([CH3:12])[C:10](=[O:11])[C:5]=2[C:4]=1[C:19]([O:21][CH3:22])=[O:20].C[S:24][C:25]1[S:26][C:27]2[CH:33]=[CH:32][CH:31]=[CH:30][C:28]=2[N:29]=1>COCCOCCOC>[CH3:12][N:9]1[C:10](=[O:11])[C:5]2[C:4]([C:19]([O:21][CH3:22])=[O:20])=[C:3]([CH2:2][N:29]3[C:28]4[CH:30]=[CH:31][CH:32]=[CH:33][C:27]=4[S:26][C:25]3=[S:24])[S:18][C:6]=2[N:7]([CH2:14][CH:15]([CH3:17])[CH3:16])[C:8]1=[O:13]参加物
4
反応物 2
生成物 1
試薬・触媒・溶媒 1
実験手順
A solution of the product of example 3 step b) (300 mg) and 2-methylthiobenzothiazole (300 mg) in diglyme (3 ml) was heated by microwave irradiation (600 W) to 160° C. After 30 min the solvent was removed by vacuum distillation and the residue purified by gradient chromatography eluting with a gradient of dichloromethane to 5% methanol in dichloromethane to give the sub-title compound as a white solid (150 mg). δ 1HCDCl3 0.93 (6H,d), 2.22 (1H,non), 3.38 (3H,s), 3.71 (2H,d), 4.00 (3H,s), 4.80 (2H,s), 7.33 (1H,dt), 7.45 (1H,dt), 7.77 (1H,dd), 7.92 (1H,d).