The invention belongs to the technical field of
chemical synthesis, and particularly relates to a preparation method of 1-(5-methoxy-2, 3-dihydro-1, 4-benzodioxane-8-yl) ethanone. Comprising the following steps: cuprous
cyanide and an initial
raw material are added into N, N-
dimethylformamide for
nitrogen displacement, and the initial
raw material is 5-bromo-8-methoxy-2, 3-dihydro-benzo [1, 4] dioxin or 5-chloro-8-methoxy-2, 3-dihydro-benzo [1, 4] dioxin; cooling after the reaction, adding
ammonia water, extracting, combining organic phases, and purifying to obtain 5-cyano-8-methoxy-2, 3-dihydro-benzo [1, 4] dioxin; the preparation method comprises the following steps: reacting 5-cyano-8-methoxy-2, 3-dihydro-benzo [1, 4] dioxin with
anhydrous tetrahydrofuran, dropwise adding a
tetrahydrofuran solution of a methyl
Grignard reagent, and reacting until no 5-cyano-8-methoxy-2, 3-dihydro-benzo [1, 4] dioxin exists; the method comprises the following steps of: extracting, concentrating and
drying, and purifying to obtain the 1-(5-methoxy-2, 3-dihydro-1, 4-benzodioxane-8-yl) ethanone, namely the 1-(5-methoxy-2, 3-dihydro-1, 4-benzodioxane-8-yl) ethanone. The method has the advantages of easily available raw materials, stable process and simple operation. The method can be applied to
isotope labeling synthesis of C13 and C14 compounds.