HRID407841

反应详情

EQUATION

反应方程式

HRID 407841 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of (1RS, 2SR,6RS,7SR)-4-bromo-5-methoxy-10-oxatricyclo[5.2.1.02,6]dec-4-en-3-one (0.315 g, 1.2 mmol), 2,6-diethyl-4-methylphenylboronic acid (0.35 g, 1.8 mmol), 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (20 mg, 0.048 mmol), palladium (II)acetate (5.5 mg, 0.024 mmol) and potassium phosphate (0.51 g, 2.4 mmol) are heated in degassed toluene at 95° C. for 24 hours. The reaction mixture is partitioned between dichloromethane and water, and the organic phase is dried over anhydrous magnesium sulfate, filtered and the filtrate is evaporated under reduced pressure. The residue is purified by column chromatography on silica gel to give (1RS,2SR,6RS,7SR)-4-(2,6-diethyl-4-methylphenyl)-5-methoxy-10-oxatricyclo[5.2.1.02,6]dec-4-en-3-one.

WORKUP

后处理

  1. customThe reaction mixture is partitioned between dichloromethane and water
  2. dry with materialthe organic phase is dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. customthe filtrate is evaporated under reduced pressure
  5. customThe residue is purified by column chromatography on silica gel