反应详情

温度

125 °C

A mixture of styrene oxide (2.40 g, 0.020 mol) and 2-amino-1-phenylethanol (4.11 g, 0.030 mol) was heated in an oil bath at 125° C. for 3 hours. The reaction mixture was cooled, dissolved in 15 mL of methanol, and the solution poured into 100 mL of water. The mixture was extracted with 2×75 mL portions of methylene chloride, the extracts combined, dried (magnesium sulfate) and concentrated to give a yellow oil that showed several products on tlc analysis. To purify, the oil was dissolved in methylene chloride (50 mL) and extracted with 2×50 mL portions of 1N HCl solution. A precipitate appeared in the methylene chloride layer which was collected and shown by mass spectral analysis to be the product. NMR analysis showed the solid to be the hydrochloride salt. The solid (0.48 g, 6% yield) was recrystallized from methanol-isopropyl ether; mp 206°-208° C. This compound is reported in Arch Pharm 293, 27-28 (1960) (CA 54:18417 g).

1. temperatureThe reaction mixture was cooled
2. extractionThe mixture was extracted with 2×75 mL portions of methylene chloride
3. dry with materialdried (magnesium sulfate)
4. concentrationconcentrated
5. customto give a yellow oil that
6. customTo purify
7. dissolutionthe oil was dissolved in methylene chloride (50 mL)
8. extractionextracted with 2×50 mL portions of 1N HCl solution
9. customwas collected