Compound in category of aryl methylamino dithio formic ether, preparation method and application
An aminodithiocarboxylic acid and ester compound technology, which can be used in the directions of heterocyclic compound active ingredients, ester active ingredients, drug combinations, etc., and can solve the problem of little anti-tumor activity.
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Embodiment 1
[0042] The preparation of embodiment 1 compound 1
[0043]
[0044] (compound 1)
[0045] 2-Fufurylamine (0.49g, 5×10 -3 mol) was dissolved in acetone (or dimethylformamide) (5mL), and anhydrous potassium phosphate (1.06g, 5×10 -3 mol), carbon disulfide (1mL, excess), after 30min, add 2-bromoacetaldehyde diethyl acetal (0.99g, 5×10 -3 mol) of acetone solution. After stirring at room temperature for 2 h, the reaction was stopped. After filtration, the filtrate was concentrated, 20 mL of water was added, and extracted with ethyl acetate. The ethyl acetate layer was washed with water and dried with anhydrous calcium chloride, then concentrated by rotary evaporation to obtain light yellow liquid compound 1 (1.32 g, 91%).
[0046] Elemental Analysis: C 12 h 19 NO 3 S 2 Calculated (%): C 49.80, H 6.62, N 4.84; Found (%): C 49.56, H 6.50, N 5.12. 1 H-NMR (CDCl 3 , δ): 1.18(t, 6H), 3.29(d, 2H), 3.52~3.75(m, 4H), 4.64(t, 1H), 4.86(d, 2H), 6.34~6.36(m, 2H), 7.38 (t, 1H), ...
Embodiment 2
[0047] The preparation of embodiment 2 compound 2
[0048]
[0049] (compound 2)
[0050] The synthesis and post-treatment methods of compound 2 are the same as those of compound 1, except that 2-bromoacetaldehyde diethyl acetal is replaced by o-chlorobenzyl chloride.
[0051] Yield: 93%, pale yellow liquid. Elemental Analysis: C 13 h 12 ClNOS 2 Calculated (%): C 52.43, H 4.06, N 4.70; Found (%): C 52.64, H 4.46, N 5.01. 1 H-NMR (CDCl 3 , δ) 4.58-4.88 (m, 2H), 6.31-6.34 (m, 2H), 7.17-7.56 (m, 7H).
Embodiment 3
[0052] The preparation of embodiment 3 compound 3
[0053]
[0054] (compound 3)
[0055] The synthesis and post-treatment methods of compound 3 are the same as those of compound 1, except that 2-bromoacetaldehyde diethyl acetal is replaced by monochloroacetone.
[0056] Yield: 96%. Rhombic white crystal, mp 75~77℃. Elemental Analysis: C 9 h 11 NO 2 S 2 Calculated (%): C 47.14, H 4.83, N 6.11; found (%): C 47.38, H 4.82, N 6.18. FAB(MH + ): calculated value 230.3; measured value 230.1.
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Abstract
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