反应详情

温度

80 °C

To methanesulfonic acid 2-benzo[b]thiophen-2-yl-ethyl ester (2.93 mmol) was added dimethylamine (30 mL, 2M in EtOH) and the mixture was heated in a sealed flask for 2 hrs at 80° C. Monitoring by TLC indicated complete conversion and the mixture was concentrated in vacuo. The residue was dissolved in EtOAc, washed with sat. NaHCO3 (2×) and subsequently extracted with 1N HCl (3×). The combined HCl layers were made basic with sat. NaHCO3, extracted with EtOAc (4×) and the combined organic layers were washed with brine, dried over MgSO4, filtered and concentrated in vacuo to give Compound 1a (2-Benzo[b]thiophen-2-yl-ethyl)-dimethyl-amine (561 mg, 94%) as a tan solid; MS(MH+)=206.

1. concentrationthe mixture was concentrated in vacuo
2. dissolutionThe residue was dissolved in EtOAc
3. washwashed with sat. NaHCO3 (2×)
4. extractionsubsequently extracted with 1N HCl (3×)
5. extractionextracted with EtOAc (4×)
6. washthe combined organic layers were washed with brine
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated in vacuo