反应详情

A mixture of 5-chloroacetyl-2,3-dihydrobenzofuran (176.2 g--see Preparation 18), 3-(S)-(-)-(1-carbamoyl-1,1-diphenylmethyl)pyrrolidine (335.0 g--see Preparation 10(B)) and potassium carbonate (335 g) were stirred in industrial methylate spirits at room temperature for 18 hours then concentrated in vacuo. The oily solid was partitioned between methylene chloride (2,500 ml) and water (2,500 ml) and the organic phase was concentrated to an oil in vacuo. The oil was dissolved in ethyl acetate (3,350 ml) and acidified with hydrochloric acid dissolved in isopropyl alcohol (180.6 ml at 24% w/v). Filtration produced the title compound as a hygroscopic solid, yield 467 g.

1. concentrationthen concentrated in vacuo
2. customThe oily solid was partitioned between methylene chloride (2,500 ml) and water (2,500 ml)
3. concentrationthe organic phase was concentrated to an oil in vacuo
4. dissolutionThe oil was dissolved in ethyl acetate (3,350 ml)
5. dissolutiondissolved in isopropyl alcohol (180.6 ml at 24% w/v)
6. filtrationFiltration