反应详情

A solution of 24b (295 mg, 0.60 mmol), 27 (258 mg, 0.9 mmol), Pd2(dba)3.CHCl3 (120 mg, 0.12 mmol), PPh3 (60 mg, 0.24 mmol), LiCl (74 mg, 1.8 mmol) and CuI (23 mg, 0.12 mmol) in dioxane (25 mL) was refluxed for one hour. The solvent was evaporated and the crude dissolved in CH2Cl2. The organic solution was extracted three times with 4N HCl solution. The aqueous solutions were basified together with solid NaHCO3 and extracted with CH2Cl2. The organic solution was evaporated and the mixture was purified by flash column chromatography. Elution with CH2Cl2/MeOH (99/1) gave 23b (66 mg, 28%) and with CH2Cl2/MeOH (9/1) gave 25 (209 mg, 71%) as a yellow solid.

1. customThe solvent was evaporated
2. dissolutionthe crude dissolved in CH2Cl2
3. extractionThe organic solution was extracted three times with 4N HCl solution
4. extractionextracted with CH2Cl2
5. customThe organic solution was evaporated
6. customthe mixture was purified by flash column chromatography
7. washElution with CH2Cl2/MeOH (99/1)