Process for preparing telmisartan
A technology of telmisartan and alkyl, which is applied in the field of preparation of telmisartan intermediates, can solve the problems that the final product is difficult to filter, wash and separate
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[0111] Another preferred aspect of the present invention is the following method for preparing intermediates of telmisartan derivatives, the intermediates of said telmisartan derivatives are substituted in 4'-[(2-n-propyl-4- The 2-position of the biphenyl group of methyl-6-(1-methylbenzimidazol-2-yl)-benzimidazol-1-yl)-methyl]-biphenyl, these derivatives are represented by formula 3" Representative, the method includes the following steps:
[0112] a) alkylating compound 11" to form compound 10", and
[0113]
[0114] b) condensation to form compound 3"
[0115]
[0116] 10″or R9″(R 4 =H)
[0117] in
[0118] R 1 is C 1 -C 6 alkyl,
[0119] R 2 is C 1 -C 6 alkyl,
[0120] R 3 is C 1 -C 6 alkyl,
[0121] R 4 is CONR 5 , where R 5 is H or C 1 -C 3 alkyl,
[0122] Z is a group capable of being converted into a tetrazolyl or carboxyl, which may be selected from CN and COR 6 , where R 6 Can be N(R) 2 OR 1 , where R is H, C 1 -C 6 alkyl or benzyl, a...
Embodiment 1
[0267] Preparation of N-(2-aminophenyl)-4-(butanylamino)-N,3-dimethyl-5-nitrobenzamide (compound 7):
[0268] To 3.9g (20mmol) N-methylbenzene-1,2-diamine dihydrochloride and 10ml CH 2 Cl 2Add 1.6ml of pyridine (20mmol) to the mixture, and stir at room temperature to obtain a free N-methylbenzene-1,2-diamine solution. The resulting solution was added to a mixture of 2.66 g (10 mmol) of compound 8, 3.24 g (20 mmol) of CDI and 60 ml of THF, stirred for 3 h and filtered. The wet filter cake was dried in an oven to obtain 2.26 g of solid compound 7 (yield: 61%).
[0269] 1 H NMR (300MHz, DMSO-d 6 ): δ8.33(s, 1H), 8.19(s, 1H), 7.11(d, 2H, J=6.9Hz), 6.63(d, 2H, J=7.8Hz), 2.70(s, 3H), 2.30 ~2.36(m, 5H), 1.60(m, 2H), 0.93(t, 3H, J=7.5Hz); ESI-MS: 369[M-1] -
Embodiment 2
[0271] Preparation of N-(2-methyl-4-(1-methyl-1H-benzo[d]imidazol-2-yl)-6-nitrophenyl)butanamide (compound 6):
[0272] A mixture of 370 mg (1 mmol) of compound 7 and 5 ml of pyridine was heated to reflux and stirred for 5 h. The mixture was diluted with ethyl acetate, washed with water, Na 2 SO 4 After drying and filtering, the solvent was removed under vacuum to obtain 0.3 g of compound 6 (yield: 85%).
[0273] ESI-MS: 353[M+1] +
PUM
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