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. 17701-61-0, name is Benzyl 3-hydroxy-2,2-dimethylpropanoate, molecular formula is C12H16O3, 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: 17701-61-0
tert-Butyl phthalate (5.38 g) was dissolved in toluene (50 ml). To this solution were successively added triethylamine (3.7 ml) and diphenylphosphoryl azide (5.7 ml) and the mixture was heated to 130C and stirred for 1 hr. The reaction mixture was allowed to cool to room temperature and 3-hydroxy-2,2-dimethylpropionic acid benzyl ester obtained in Example 1-4 a) (4.95 g) was added. The mixture was stirred at room temperature for 17 hr. The reaction mixture was diluted with ethyl acetate (50 ml), washed successively with water (50 ml) and saturated aqueous sodium chloride solution (5 ml), dried and concentrated under reduced pressure. The obtained oily substance was purified by silica gel column chromatography (n-hexane/ethyl acetate=1:1). The oily substance (3.28 g) after purification was dissolved in dichloromethane (30 ml). This solution was cooled to 0C and trifluoroacetic acid (30 ml) was added. The mixture was heated to room temperature and stirred for 3 hr. The reaction mixture was concentrated under reduced pressure, after which water (50 ml) was added, and the mixture was extracted with ethyl acetate (150 ml). The organic layer was washed successively with water (50 ml×3) and saturated aqueous sodium chloride solution (50 ml), dried and concentrated under reduced pressure. The obtained oily substance was purified by column chromatography to give the title compound (2.54 g, yield 89%) as a colorless oil.1H-NMR(delta, 300MHz, DMSO-d6) 1.22(6H,s),4.20(2H,s), 5.13(2H,s),7.12(1H,m),7.25-7.34 (5H,m),7.60(1H,m), 7.99(1H,dd,J=1.6,7.9Hz),8.23(1H,d,J=7.9Hz),10.72(1H,s),13.63(1 H,brs).
With the rapid development of chemical substances, we look forward to future research findings about 17701-61-0.
Reference:
Patent; Japan Tobacco Inc.; EP1452526; (2004); A1;,
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