反应详情

To a 3-L reaction vessel was charged and stirred potassium carbonate (152 g), 3-hydroxybenzaldehyde (67.6 g), dimethylformamide (DMF, 250 mL) and 3-chloropropyl phenylmethyl ether (96.4 g) at 90° C. for ˜18 h. Water (567 mL) was added followed by tert-butyl methyl ether (907 mL). The bottom aqueous layer was separated and the organic layer washed with 1N sodium hydroxide (2×567 mL) and water (1×567 mL). The organic solution was concentrated to a minimum after which ethanol (200 proof, 907 mL) was added and the solution concentrated to a minimum and filtered though a 1-μm filter.

1. additionwas charged
2. customThe bottom aqueous layer was separated
3. washthe organic layer washed with 1N sodium hydroxide (2×567 mL) and water (1×567 mL)
4. concentrationThe organic solution was concentrated to a minimum after which ethanol (200 proof, 907 mL)
5. additionwas added
6. concentrationthe solution concentrated to a minimum
7. filtrationfiltered though a 1-μm
8. filtrationfilter