反应详情

To a solution of 1-methylisoquinoline (133 μL, 1.0 mmol) in THF under nitrogen was added dropwise a solution of LiBEt3H in THF (1.0M, 2.2 mL, 2.2 mmol) to give a yellow solution. After stirring 1.5 h, MeOH (1.2 mL) was added dropwise to produce a clear colorless solution, which was then diluted with 1M aq. HCl and ether. The aqueous layer was extracted three times with ether, then made basic (pH 14) by addition of 1M aq. NaOH. The aqueous layer was extracted five times with DCM, dried over MgSO4, filtered and concentrated to give the desired product in 77% yield, which was used without further purification. LC/MS (10-99%) M/Z: M+1 obs=148.3; tR=0.62 min.

1. customto give a yellow solution
2. customto produce a clear colorless solution, which
3. extractionThe aqueous layer was extracted three times with ether
4. additionby addition of 1M aq. NaOH
5. extractionThe aqueous layer was extracted five times with DCM
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated