New amine compounds and their use in the treatment of depression
A technology of compounds, drugs, applied in the field of medicine
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Embodiment 1
[0069] Example 1 5-(3-Methylamino-1-thiophen-2-yl)-propyl-benzo[1,3]dioxa-4-ol hydrochloride (I 1 ) preparation
[0070]
[0071] 1.1 Preparation of 3-dimethylamino-1-(thiophen-2-yl)-propyl-1-one hydrochloride
[0072] Place 20.0g (0.16mol) of 2-acetylthiophene, 16.8g (0.21mol) of dimethylamine hydrochloride, 9.5g (0.32mol) of paraformaldehyde and 50mL of absolute ethanol in a 150mL three-necked flask, and add concentrated Hydrochloric acid to pH 3-4, heated to reflux for 8h. Stop the reaction, cool to room temperature naturally, refrigerate overnight, filter with suction, wash the filter cake with cold absolute ethanol until white, and obtain 31.2 g of white crystals, with a yield of 89.6%. MS(m / e): 184.3(M+1 + ).
[0073] 1.2 Preparation of 3-dimethylamino-1-(thiophen-2-yl)-propanol
[0074] Dissolve 30.8g (0.14mol) of 3-dimethylamino-1-(2-thienyl)-propyl-1-one hydrochloride in 150mL distilled water, add dropwise 2.5M sodium hydroxide aqueous solution until the pH ...
Embodiment 2
[0082] Example 2 7-(3-Methylamino-1-thiophene-2-propyl)-benzo[1,3]dioxol-4-ol hydrochloride (II 1 ) of the preparation of the preparation
[0083]
[0084] Add 2 g (6.85 mmol) of N-methyl-3-(benzo[1,3]dioxol-4-oxyl)-3-(thiophen-2-yl)-propylamine to 40 mL of ethyl acetate , add 0.8g concentrated hydrochloric acid under stirring condition, stir at room temperature for 1h, heat the system to 45°C, continue the reaction for 1h, distill off the solvent under reduced pressure, separate by column chromatography, and separate by silica gel column chromatography to obtain a light yellow solid 7-(3-formazan Amino-1-thiophene-2-propyl)-benzo[1,3]dioxol-4-phenol hydrochloride (Ⅱ 1 ) 0.35g, yield 17.5%. MS (m / e): 292.2 (M+H + ). 1 H-NMRδ (ppm, DMSO-d 6 ): 9.27(br s,3H); 7.32-7.35(m,1H); 6.97-6.99(m,2H); 6.43-6.48(d,,1H); 6.33-6.38(d,1H); (m, 2H); 4.52-4.65(t, 1H); 2.73-2.77(m, 2H); 2.43(s, 3H); 2.31-2.33(m, 2H).
Embodiment 3
[0085] Example 3 5-(3-Ethylamino-1-thiophene-2-propyl)-benzo[1,3]dioxol-4-phenol hydrochloride (I 2 ) preparation
[0086]
[0087] Operation is the same as in Example 1, with N-ethyl-3-(benzo[1,3]dioxacyclo-4-oxyl group)-3-(thiophen-2-yl)-propylamine (see Chinese patent for preparation method) ZL200810127171.5) as the starting material to obtain light yellow solid 5-(3-ethylamino-1-thiophene-2-propyl)-benzo[1,3]dioxol-4-phenol hydrochloride ( I 2 )0.24g, yield 33.5%. MS (m / e): 306.2 (M+H + ). 1 H-NMRδ (ppm, DMSO-d 6 ): 9.01(br s,3H); 7.33-7.37(m,1H); 7.25-7.26(dd,1H); 6.97-6.98(d,1H); 6.63-6.65(d,,1H); 6.47-6.49 (d,2H);5.95-5.97(m,2H);4.58-4.62(t,1H);2.34-2.54(m,3H);2.06-2.12(m,1H);1.86-1.92(m,1H) ;0.80-0.84(t,3H).
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