反应详情

To a stirred solution of 4-hydroxymethyl-2-(2-methylphenyl)benzoic acid methyl ester prepared in Example 331A (10.85 g, 42.2 mmol) in dry DMF (40 mL) at 0° C. was added successively lithium bromide (4.00 g, 46.6 mmol, 1.1 eq) and phosphorus tribromide (4.18 mL, 44.5 mmol, 1.05 eq) at a rate such that the temperature did not exceed 5° C. On completion of the addition the mixture was warmed to ambient temperature, and quenched by the addition of ice. The resultant solution was partitioned between water and ether; the ethereal solution was dried (Na2SO4), filtered and the solvent removed under reduced pressure to afford the title compound (13 g, 96%) as a colorless oil.

1. customdid not exceed 5° C
2. additionOn completion of the addition the mixture
3. customquenched by the addition of ice
4. customThe resultant solution was partitioned between water and ether
5. dry with materialthe ethereal solution was dried (Na2SO4)
6. filtrationfiltered
7. customthe solvent removed under reduced pressure