反应详情

A solution of 8.27 gm (33.75 mmol) of 3-bromo-2,5-dimethoxy benzaldehyde* in 40 ml THF and 20 ml water was cooled to 10° C. and treated portionwise with 3.83 gm (101.2 mmol) NaBH4. Stirring was maintained at ambient temperature until tlc analysis (silica gel; 1:4 ethyl acetate:hexane) indicated the absence of starting aldehyde. After 30 minutes the solvent was removed in vacuo and the residue was portioned between ethyl acetate and water. After washing with brine and drying (Na2SO4), the ethyl acetate extract was concentrated in vacuo to yield 8.34 gm (99%) of a white solid, mp 59°-60° C.; tlc (cited), Rf 0.12.

1. customAfter 30 minutes the solvent was removed in vacuo
2. washAfter washing with brine
3. dry with materialdrying (Na2SO4)
4. extractionthe ethyl acetate extract
5. concentrationwas concentrated in vacuo