Catenated ring compound serving as protein degradation agent as well as preparation method and application of catenated ring compound
A compound, cycloalkyl technology, applied in the field of compound and its preparation and application as a protein degrading agent, can solve problems such as not necessarily applicable
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reference example 1
[0149] Reference Example 1: Preparation of Intermediate I-1
[0150]
[0151] [1-(4-Bromophenyl)-cyclopropyl] tert-butyl carbamate (950mg, 3.05mmol), 4-methylthiazole (605mg, 6.1mmol), potassium acetate (600mg, 6.1mmol) and acetic acid Palladium (34mg, 0.153mmol) was mixed in N,N-dimethylacetamide (10mL), heated to 130°C under nitrogen atmosphere, and stirred for 8 hours. The reaction solution was cooled to room temperature, diluted with ethyl acetate (20 mL), filtered, the filtrate was diluted with water (60 mL), extracted with ethyl acetate (20 mL×3), the organic phases were combined, dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated under reduced pressure and purified by silica gel chromatography to obtain intermediate I-1.
[0152] LC-MS(ESI)[M+H] + 331.3.
reference example 2
[0153] Reference Example 2: Preparation of Intermediate I-2
[0154]
[0155] Intermediate I-1 (370mg, 1.12mmol) was dissolved in hydrogen chloride methanol solution (20mL, 4M), and stirred at room temperature for 4 hours. The reaction solution was concentrated, neutralized by adding saturated aqueous sodium bicarbonate solution, extracted with dichloromethane (20 mL×3), the organic phases were combined, dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated under reduced pressure to obtain intermediate I-2. The crude product was directly used in the next reaction without further purification.
[0156] LC-MS(ESI)[M+H] + 231.1.
reference example 3
[0157] Reference Example 3: Preparation of Intermediate I-3
[0158]
[0159] Intermediate I-2 (240mg), Boc-L-hydroxyproline (240mg, 1.04mmol), N,N-diisopropylethylamine (400mg, 3.12mmol) mixed in N,N-dimethylformaldehyde Add O-(7-azabenzotriazol-1-yl)-N,N,N'-tetramethyluronium hexafluorophosphate (600mg, 1.56mmol) to amide (4mL), and stir the reaction at room temperature 16 hours. The reaction solution was diluted with water (20 mL), extracted with ethyl acetate (20 mL×3), the organic phases were combined, dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated under reduced pressure and purified by silica gel chromatography to obtain intermediate I-3.
[0160] LC-MS(ESI)[M+H] + 444.3.
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