Water → HCID 70049825, compound

Participants

Reaction Steps

2.17 g (6.17 mmol) of trans-3-(3,5-difluoro-2-methoxybenzyl)-4-(3,4-dimethoxyphenyl)pyrrolidine prepared in step (13) of Example 4 was dissolved in 30 ml of chloroform, and 0.75 g (7.4 mmol) of triethylamine was added thereto. 10 ml of a solution of 0.5 ml (7.0 mmol) of acetyl chloride in chloroform was dropwise added thereto under cooling with ice, and the mixture was stirred at room temperature for 3 hr. 1 ml of water was added thereto to stop the reaction. The reaction mixture was washed with water, a 2N hydrochloric acid solution, and a saturated aqueous sodium hydrogencarbonate solution sequentially, and dried over anhydrous sodium sulfate. The solvent was distilled off in vacuo, and the residue was subjected to silica gel column chromatography (methylene chloride:methanol=97:3) to prepare 2.5 g (quantitative) of the intended product.

Provenance & Evidence