Kallikrein 7 small-molecule inhibitor as well as preparation method and application thereof
A technology of small molecule inhibitors and kallikrein, which is applied in skin diseases, organic chemistry, drug combination, etc., can solve the problems of limited effect, fast degradation speed, and inability to penetrate the stratum corneum of the skin, so as to achieve convenient operation and absorption Fast, inhibits the effect of KLK7
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Embodiment 1
[0041] Example 1: Preparation of Kallikrein 7 Small Molecule Inhibitors
[0042] 1.0mol compound (Ⅱ) was dissolved in 2.0mol concentrated H 2 SO 4 In, add dropwise 1.0mol concentrated H 2 SO 4 with 1.0mol concentrated HNO 3 The formed mixed acid was controlled at a temperature below 30° C. and reacted for 4 hours to obtain compound (Ⅲ), poured into ice water, filtered to obtain crude compound (Ⅲ), and separated by column to obtain compound (Ⅲ).
[0043] Add 25 mol of water, 3.0 mol of iron powder, 0.3 mol of HCl (100% hydrogen chloride, 37% concentration) in the reaction bottle, control the temperature at 90° C., add compound (Ⅲ) in batches, react for 3 hours, neutralize with sodium carbonate, pass Compound (Ⅳ) was obtained by column separation.
[0044]Add compound (Ⅳ), ether, triethylamine to the reaction flask, then add succinoyl chloride dropwise, react at room temperature for 2 hours, compound (Ⅳ): ether: triethylamine: succinoyl chloride = 1:5:2.5:1 (molar ratio), ...
Embodiment 2
[0051] Example 2: Preparation of Kallikrein 7 Small Molecule Inhibitors
[0052] 1.0mol compound (Ⅱ) was dissolved in 2.0mol concentrated H 2 SO 4 In, add dropwise 1.0mol concentrated H 2 SO 4 with 1.0mol concentrated HNO 3 The formed mixed acid was controlled at a temperature below 30° C., and reacted for 6 hours to obtain compound (Ⅲ), which was poured into ice water, filtered to obtain crude compound (Ⅲ), and separated by column to obtain compound (Ⅲ).
[0053] Add 20 mol of water, 2.0 mol of iron powder, 0.1 mol of HCl (100% hydrogen chloride, 37% concentration) in the reaction bottle, control the temperature at 90°C, add compound (Ⅲ) in batches, react for 2 hours, neutralize with sodium carbonate, pass Compound (Ⅳ) was obtained by column separation.
[0054] Add compound (Ⅳ), diethyl ether and triethylamine to the reaction flask, then add succinoyl chloride dropwise, and react at room temperature for 2 hours, compound (Ⅳ): ether: triethylamine: succinoyl chloride=0.5...
Embodiment 3
[0060] Example 3: Preparation of Kallikrein 7 Small Molecule Inhibitors
[0061] 1.0mol compound (Ⅱ) was dissolved in 2.0mol concentrated H 2 SO 4 In, add dropwise 1.0mol concentrated H 2 SO 4 with 1.0mol concentrated HNO 3 The formed mixed acid was controlled at a temperature below 30° C., and reacted for 6 hours to obtain compound (Ⅲ), which was poured into ice water, filtered to obtain crude compound (Ⅲ), and separated by column to obtain compound (Ⅲ).
[0062] Add 30 mol of water, 5 mol of iron powder, 0.5 mol of HCl (100% hydrogen chloride, 37% concentration) into the reaction bottle, control the temperature at 90°C, add compound (Ⅲ) in batches, react for 3 hours, neutralize with sodium carbonate, and pass through the column Compound (IV) was isolated.
[0063] Add compound (Ⅳ), ether, triethylamine to the reaction flask, then add succinoyl chloride dropwise, react at room temperature for 2 hours, compound (Ⅳ): ether: triethylamine: succinoyl chloride = 2:6:3.5:2 (m...
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