反应详情

To solution of tert-butyl 3-(5-butyryl-1-methyl-1H-indol-2-yl)pyrrolidine-1-carboxylate (0.823 g, 2.22 mmol) in DCM (5 mL) was added 2,4-dimethoxybenzylamine (0.38 mL, 2.53 mmol) and NEt3 (0.90 mL, 6.45 mmol). Mixture was cooled to 0° C. before TiCl4 solution (1M DCM, 1.45 mL, 1.45 mmol) was added dropwise via syringe pump over 30 min. Reaction was allowed to warm to room temperature and stirred overnight. Mixture was diluted with DCM (10 mL) and then quenched with NaHCO3 (aqueous saturated, 10 mL). Upon vigorous shaking organic phase was separated using a PTFE phase separator, dried over Na2SO4. Removal of the solvent afforded product (1.15 g, quant) as yellow oil, which was taken directly into next steps without purification.

1. additionwas added dropwise via syringe pump over 30 min
2. customReaction
3. customquenched with NaHCO3 (aqueous saturated, 10 mL)
4. customUpon vigorous shaking organic phase was separated
5. dry with materialdried over Na2SO4
6. customRemoval of the solvent
7. customafforded product (1.15 g, quant) as yellow oil, which
8. customwas taken directly into next steps without purification