Hexamethylcyclotrisiloxane application is a kind of great application value of structural unit, widely exists in spices, pesticides, coal tar, essential oils and dyes. As an important pharmaceutical intermediate and fine chemical raw material, 2-pyridine methanol is widely used and has a broad market development. In medicine, as an important medical intermediate, 2-pyridinyl alcohol can be used for the synthesis of blood exchange than xacidine, and is also the raw material for the synthesis of organophosphate antidotes.
In the preparation of (4-methoxy-pyridine-2-yl) methanol, the literature first crystallized 4-methoxy-2-hydroxymethylpyridine-trifluoroacetate with toluene/ethyl acetate mixed solvent, obtained 4-methoxy-2-hydroxymethylpyridine-trifluoroacetate and then synthesized (4-methoxy-pyridine-2-yl) methanol by potassium carbonate, with low yield. In this study, crude 4-methoxy-2-hydroxymethylpyridine trifluoroacetate was directly prepared (4-methoxy-pyridine 2-yl) methanol without purification. After treatment, activated carbon and neutral alumina were used for decolorization. The yield was improved and it could be used for commercial production.
Add MTBE(20 ml), heat to 50℃, then add n-heptane (80 ml), brown solid gradually precipitation, cool to 0℃, stir for 2 hours, filter, filter cake with cold n-heptane (20 ml) washing, brown solid (4-methoxy-pyridine-2-yl) methanol. Purity was determined by HPLC.
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