反应详情

The 5-bromo-2-hydroxybenzaldehyde (4.00 g, 19.9 mmol) in Et2O (40.0 mL) and THF (10.0 mL) was added dropwise to the isopropylmagnesium chloride (2 M in Et2O, 29.8 mL, 59.7 mmol) at ambient temperature. The reaction was stirred for about 15 min then MeOH (5 mL) was added followed by saturated aqueous NH4Cl and 1 N HCl. The reaction was extracted with EtOAc and then the combined organic layers were extracted with brine, dried over MgSO4, filtered, and evaporated to give the title compound as an oil (5.96 g, >100% yield). NMR showed some EtOAc but it was used as is the next step: 1H NMR (DMSO-d6, δ) 0.87 (3H, d), 1.03 (3H, d), 2.06 (1H, m), 2.77 (1H, s), 4.49 (1H, d), 6.78 (1H, d), 7.02 (1H, s), 7.25 (1H, dd), 8.11 (1H, s)

1. extractionThe reaction was extracted with EtOAc
2. extractionthe combined organic layers were extracted with brine
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. customevaporated