HRID733388
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a suspension of 4-bromo-2-phenoxybenzoic acid, 2a (35.1 g, 120 mmol) in. methylene chloride (350 mL) at 0° C. was added dropwise trifluoroacetic anhydride (20.3 mL, 144 mmol), and the reaction was stirred for 15 min. Boron trifluoride diethyl etherate (1.46 mL, 12.0 mmol) was added dropwise. The reaction became homogeneous upon stirring for 1 h at rt. The reaction was poured into 1 N NaOH, and the organic phase was dried over magnesium sulfate, filtered, and concentrated to give title compound 3-bromo-xanthen-9-one, 3a (32.14 g, 116 mmol). MS m/z (MH+) 275.
WORKUP
后处理
- stirringupon stirring for 1 h at rt
- dry with materialthe organic phase was dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated