反应详情

温度

0 °C

Under an argon atmosphere, 5.005 g (6.458 mmol) of the compound from example 32A were dissolved in 355 ml of tetrahydrofuran and cooled to 0° C., and 16.145 ml (16.145 mmol) of a 1N solution of bis(trimethylsilyl)sodium amide in tetrahydrofuran were added dropwise. The mixture was stirred at 0° C. for 2 h and then at RT for 16 h. 16.145 ml (16.145 mmol) of 1N hydrochloric acid were added and the mixture was concentrated on a rotary evaporator. The residue was taken up in ethyl acetate and the organic phase was washed twice with water, dried over sodium sulfate and concentrated on a rotary evaporator. 6.13 g of the title compound were obtained (purity by HPLC 61%). 500 mg of residue were purified by means of preparative HPLC (eluent: methanol/water, gradient 30:70→90:10). 93 mg of the title compound were obtained (36% of theory).

1. waitat RT for 16 h
2. concentrationthe mixture was concentrated on a rotary evaporator
3. washthe organic phase was washed twice with water
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated on a rotary evaporator