Synthetic Route of 7270-63-5, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 7270-63-5 name is 5-Diazo-2,2-dimethyl-1,3-dioxane-4,6-dione, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
General procedure: 1- (3,4,5-trimethoxyphenyl) hexan-1-one (3aa) (53.3 mg, 0.2 mmol, 100 mol%),[IrCp * Cl 2] 2 (3.2 mg, 0.004 mmol, 2 mol%) or[RhCp * Cl 2] 2 (2.5 mg, 0.004 mmol, 2 mol%),AgNTf2 (6.2 mg, 0.016 mmol, 8 mol%),AgOAc (2.6 mg, 0.016 mmol, 8 mol%) andIn an oven-dried sealed tube filled with 5-diazo-2,2-dimethyl-1,3-dioxane-4,6-dione (4a) (40.8 mg, 0.24 mmol, 120 mol%), EtOH (18.4 mg, 0.4 mmol, 200 mol%) and DCE (1 mL) were added in air at room temperature.The reaction mixture was stirred at 60 C for 20 h. The reaction mixture was cooled to rt, diluted with EtOAc (3 mL) and concentrated in vacuo. The residue was purified by flash column chromatography (n-hexane / EtOAc = 12: 1) to give 5aa (50.2 mg, 71%) as a yellow solid.
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-Diazo-2,2-dimethyl-1,3-dioxane-4,6-dione, and friends who are interested can also refer to it.
Reference:
Patent; SUNGKYUNKWAN University Research & Business Foundation; Kim In-su; Kim Hyeong-sik; (40 pag.)KR2019/87836; (2019); A;,
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