反应详情

温度

120 °C

A mixture of 22 (50 mg, 0.079 mmol), benzenethiol (13.0 mg, 0.118 mmol), copper (I) iodide (3.0 mg, 0.016 mmol), N,N-dimethylglycine (1.62 mg, 0.016 mmol) and potassium phosphate (41.8 mg, 0.197 mmol) in DMF (0.5 mL) were heated at 120° C. for 69 h. The reaction mixture was cooled and partitioned between AcOEt/brine, the layers separated and the aqueous phase extracted with more AcOEt (2×). The combined organic extracts were dried (MgSO4) and concentrated. The resulting crude residue containing 23 was used for the subsequent deprotection step.

1. temperatureThe reaction mixture was cooled
2. custompartitioned between AcOEt/brine
3. customthe layers separated
4. extractionthe aqueous phase extracted with more AcOEt (2×)
5. dry with materialThe combined organic extracts were dried (MgSO4)
6. concentrationconcentrated
7. additionThe resulting crude residue containing 23