New benzothiazolecarboxamides
A technology of benzothiazole and formamide, which is applied in the field of treatment, new intermediates, and preparation of said compounds, can solve problems such as limitations
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Embodiment 1
[0174] N-4-tert-butylphenyl-2-methyl-1,3-benzothiazole-5-carboxamide.
[0175] 2-Methyl-1,3-benzothiazole-5-carboxylic acid (90.0 mg, 0.400 mml) was dissolved in DMF (3.00 mL), and HATU (190 mg, 0.500 mmol), 4-tert-butylaniline (75.0 mg, 0.500mmol) and Et 3 N (0.100 mL). The mixture was stirred for 3 hours, and the solvent was evaporated. The product was purified by flash chromatography on silica gel eluting with a mixture of hexanes and EtOAc (9:1 to 4:1) to afford the product (42.0 mg, 0.129 mmol, 32.0%). 1 H NMR (400MHz, DMSO-D 6)δppm 1.27 (s, 9H) 2.83 (s, 3H) 4.90-5.18 (br s, 1H) 7.36 (d, J = 8.98Hz, 2H) 7.71 (dd, J = 8.98, 2.73Hz, 2H) 7.96 (dd , J=8.40, 1.76Hz, 1H) 8.16(d, J=8.40Hz, 1H) 8.51(d, J=1.37Hz, 1H) 10.31(s, 1H); MS[M+H] calculated value 325.0, measured Value 325.0.
Embodiment 2
[0177] N-4-cyclohexylphenyl-2-methyl-1,3-benzothiazole-5-carboxamide.
[0178] 2-Methyl-1,3-benzothiazole-5-carboxylic acid (100 mg, 0.440 mml) was dissolved in DMF (5.00 mL), and HATU (190 mg, 0.500 mmol), 4-cyclohexylaniline (88.0 mg , 0.500mmol) and Et 3 N (0.100 mL). The mixture was stirred for 3 hours, and the solvent was evaporated. The product was purified by flash chromatography on silica gel eluting with a mixture of hexanes and EtOAc (9:1 to 4:1) to give nearly pure product which was recrystallized from heptane and EtOAc to give pure product (15.1 mg, 0.043 mmol, 10.0%). 1 H NMR (400MHz, DMSO-D 6 )δppm 1.15-1.50 (m, 5H) 1.60-1.83 (m, 6H) 2.82 (s, 3H) 7.18 (d, J = 8.59Hz, 2H) 7.67 (d, J = 8.59, 2H) 7.94 (dd, J =8.40, 1.76Hz, 1H) 8.14 (d, J = 8.40Hz, 1H) 8.48 (d, J = 1.56Hz, 1H) 10.30 (s, 1H); MS [M+] calculated value 350.2, measured value 351.0.
Embodiment 3
[0180] 2-Methyl-N-[2-methyl-4-trifluoromethylphenyl]-1,3-benzothiazole-5-carboxamide.
[0181] 2-Methyl-1,3-benzothiazole-5-carboxylic acid (90.0mg, 0.470mmol) and 2-methyl-4-trifluoromethylaniline (123mg, 0.700mmol), EDC (134mg, 0.700 mmol) and DMAP (85.0 mg, 0.700 mmol) were mixed in DCM (5.00 mL) and DMF (3.00 mL) for 48 hours. The mixture was concentrated and the product was purified by flash chromatography on silica gel eluting with a mixture of heptane and EtOAc (95 / 5 to 75 / 25) to give the product (14.0 mg, 0.0400 mmol, 8.50%). 1 H NMR (600MHz, chloroform-D) δppm 2.42(s, 3H) 2.89(s, 3H) 7.50(s, 1H) 7.54(d, J=8.45Hz, 1H) 7.85-8.05(m, 3H) 8.32(d , J = 8.45 Hz, 1H) 8.41 (s, 1H); MS [M+H] calcd. 351.0, found 351.0.
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