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RARECHEM AL BF 1076 synthesis

9synthesis methods
-

Yield:26409-24-5 100%

Reaction Conditions:

with potassium carbonate in acetone at 0 - 20;Inert atmosphere;

Steps:

2.b-4.iii Synthesis of Compound 22

Compound 21 (629 mg, 2.29 mmol) was placed in an eggplant-shaped flask and sufficiently dried with a vacuum pump Replaced with N 2 gas. Thereafter, 25 mL of acetone was added with a syringe, and further under N 2 gas at 0 ° C. Potassium carbonate (6.3 g, 45.8 mmol) and methyl iodide (1.42 mL, 22.9 mmol) were added and the reaction was allowed to react overnight at room temperature under N 2 gas. After the reaction, acetone was removed by an evaporator, and 50 mL of H 2 O was added to the reaction solution. Ethyl acetate was added to the aqueous layer, and partitioning extraction was carried out. The organic layer was washed with NaHCO 3 and saturated brine, dried over magnesium sulfate, filtered, and the filtrate obtained was concentrated to dryness with an evaporator. Subsequently, it was purified using silica gel column chromatography (developing solvent 8: 1 to 6: 1 hexane / ethyl acetate). Fractions containing the desired product were collected and concentrated to give Compound 22 (yield: 692 mg, yield: 100%).

References:

JP2017/43558,2017,A Location in patent:Paragraph 0080; 0083