反应详情

After dissolving 2-[(1-naphthalen-1-ylmethyl-piperidin-4-ylmethyl)-(2-trimethylsilanyl-ethoxymethyl)-amino]-1-(2-trimethylsilanyl-ethoxymethyl)-1H-benzimidazole-5-carboxylic acid methyl ester (624 mg, 0.91 mmol) in anhydrous tetrahydrofuran (10 ml) under a nitrogen stream, aluminum lithium hydride (72.4 mg, 1.82 mmol) was added at 0° C., and the mixture was stirred for 2 hours. After then adding a saturated aqueous sodium sulfate solution, extraction was performed with ethyl acetate and then with dichloromethane. Each extract was washed with saturated brine, and then combined and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain [2-[(1-naphthalen-1-ylmethyl-piperidin -4-ylmethyl)-(2-trimethylsilanyl-ethoxymethyl)-amino]-1-(2-trimethylsilanyl-ethoxymethyl)-1H-benzimidazol-5-yl]-methanol. The compound was identified by LC-MS.

1. additionwas added at 0° C.
2. additionAfter then adding
3. extractiona saturated aqueous sodium sulfate solution, extraction
4. washEach extract was washed with saturated brine
5. dry with materialdried over anhydrous sodium sulfate
6. distillationThe solvent was distilled off under reduced pressure