反应详情

温度

-30 °C

To a solution of thieno[2,3-b]pyridine (0.35 g, 2.6 mmoles) prepared according to well known methods [see, Klemm, et al. (1969) J. Org. Chem., 34:347-354; see, also U.S. Pat. Nos. 5,026,700, 4,577,014, 4,406,898, 4,375,544, 4,311,845, and 4,161,599] in THF (10 ml) at −78° C. was added t-BuLi (1.7 M, 2.0 ml, 3.4 mmoles). The reaction solution was slowly warmed to −30° C. over a 45 minute period followed by the addition of bromoethane (0.25 ml, 3.4 mmoles). The solution was stirred 2 hours at ambient temperature then diluted with EtOAc (50 ml) and washed with H2O (75 ml). The organic phase was dried (MgSO4), filtered and concentrated to collect 0.41 g (97%) of the title compound as an orange-brown oil.

1. washwashed with H2O (75 ml)
2. dry with materialThe organic phase was dried (MgSO4)
3. filtrationfiltered
4. concentrationconcentrated
5. customto collect 0.41 g (97%) of the title compound as an orange-brown oil