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. 26021-57-8, name is 3,4-Dihydro-2H-benzo[b][1,4]oxazin-6-ol, molecular formula is C8H9NO2, The 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. Recommanded Product: 26021-57-8
i) 1-(6-Hydroxy-2, 3-dihvdro-benzof1, 4loxazin-4-vl)-3-methoxy-propan-1-one A suspension of 0.58 g of 3,4-dihydro-2H-benzo [1,4] oxazin-6-ol in 25 ml of dichloromethane is treated with 0. 613 ml of pyridine and then cooled to 0C. 0.906 ml of 3- methoxypropionyl chloride are added and the reaction mixture is allowed to slowly warm to room temperature. After stirring for 2. 5 hours, the reaction mixture is concentrated by evaporation-the residue is partitioned between ethyl acetate and water. The organic phase is washed with 1 N HCI, water and brine, dried over sodium sulphate and concentrated by evaporation. The crude ester-amide intermediate is dissolved in 30 ml of methanol and treated with 1.2 ml of 1 N aqueous potassium hydroxide solution. After 2 hours, the reaction mixture is concentrated by evaporation-the residue is diluted with ethyl acetate, water and 1 N HCI. The separated organic phase is washed with water and brine, dried over sodium sulphate and concentrated by evaporation. The title compound is obtained as a light brown oil from the residue by means of flash chromatography (SiO2 60F). Rf = 0.54 (EtOAc); Rt = 2.62.
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Reference:
Patent; Speedel Experimenta AG; WO2005/37803; (2005); A1;,
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