Germatrane compound as well as preparation method and application thereof
A compound and tricyclic technology, applied in the field of azazagermanium tricyclic compounds and their preparation
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Embodiment 1
[0129] Example 1 : Preparation of 3-(2,8,9-trioxa-5-aza-1-germaniumtricyclo[3.3.3.0]undecyl)-10-hydroxy-decanoic acid
[0130] (1) Preparation of trichlorogermanium form
[0131]According to the literature (Shangguan Guoqiang, Qin Mei. Synthesis, crystal structure and vibration spectrum of carboxyethyl germanium trichloride, Journal of Qufu Normal University, 1990, 16 (4): 54-58; Shangguan Guoqiang, Zhang Shugong, Ni Jiazuan, etc. . The synthesis of β-(phenol ester group) ethyl germanium sesquioxide and its effect on in vitro cultured cells, Applied Chemistry, 1989, 6(5):59-62), 6.0 grams of germanium dioxide (0.057mol) Mix well with 12.0 grams of sodium hypophosphite (0.136mol) and put it into a 125ml three-necked flask equipped with a stirrer, add 60mL of concentrated hydrochloric acid and 15ml of distilled water to it, install a spherical condenser, and make the temperature of the reaction solution 80~ After heating and stirring at 90°C for three hours, the solution beca...
Embodiment 2
[0144] Example 2 : 3-(2,8,9-trioxa-5-aza-1-germaniumtricyclo[3.3.3.0]undecyl)-10-hydroxy-decanoic acid methyl ester
[0145]
[0146] 3-(2,8,9-Trioxa-5-aza-1-germaniumtricyclo[3.3.3.0]undecyl)-10-hydroxy-decanoic acid 0.41 g (0.001 mol) and 50 ml methanol Add it to the reaction bottle, add 5 ml of thionyl chloride dropwise at room temperature, heat and reflux for 2 h after dropping, cool to room temperature, continue stirring for 5 h, distill off methanol and remaining thionyl chloride under reduced pressure, and recrystallize from ethanol to obtain white crystals Powder 0.40 g (0.88 mmol). The yield is 88.9%, and the molecular formula is C 17 h 33 o 6 GeN has a molecular weight of 420.13. EI-MS(m / z, %):421.09[M + , 92], 220[Ge(OCH 2 CH 2 ) 3 N, 100], 160[25], 146[12], 130[5], 116[5], 100[3] .
Embodiment 3
[0147] Example 3 : Preparation of 3-(2,8,9-trioxa-5-aza-1-germaniumtricyclo[3.3.3.0]undecyl)-10-hydroxy-decylamide
[0148]
[0149] 3-(2,8,9-Trioxa-5-aza-1-germaniumtricyclo[3.3.3.0]undecyl)-10-hydroxy-decanoic acid methyl ester 0.32 g (0.77 mmol) and 28 Add 20 ml of % ammonia water into the reaction flask, stir at room temperature for 3 h, extract with dichloromethane, concentrate to dryness, and recrystallize from ethyl acetate to obtain 0.22 g (0.54 mmol) of white crystals with the molecular formula C 16 h 32 o 5 GeN 2 , the molecular weight is 405.08. EI-MS(m / z, %):406.09[M + , 91], 220[Ge(OCH 2 CH 2 ) 3 N, 100], 160[22], 146[14], 130[4], 116[5], 100[3] .
[0150] Other compounds can be prepared with reference to the above examples.
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