HRID733388

反应详情

EQUATION

反应方程式

HRID 733388 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringupon stirring for 1 h at rt
  2. dry with materialthe organic phase was dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated