反应详情

A solution of (3RS)-1-(2-acetylthiophen-3-yl)methyl-3-tert-butoxycarbonylamino-2,3-dihydro-5-isopropyl-1H-1,4-benzodiazepin-2-one (0.370 g) in ethyl acetate (50 ml) was treated with gaseous hydrogen chloride at 5˜10° C. in an ice-bath for 30 minutes. The resultant mixture was extracted with 3N aqueous hydrochloric acid (2×10 ml). The aqueous layer was basified with sodium hydrogen carbonate and extracted with ethyl acetate (2×50 ml). The extracts were combined, over sodium sulfate, filtered and concentrated in vacuo to afford (3RS)-1-(2-acetylthiophen-3-yl)methyl-3-amino-2,3-dihydro-5-isopropyl-1H-1,4-benzodiazepin-2-one (0.230 g), which was used in a following reaction step without further purification.

1. extractionThe resultant mixture was extracted with 3N aqueous hydrochloric acid (2×10 ml)
2. extractionextracted with ethyl acetate (2×50 ml)
3. filtrationfiltered
4. concentrationconcentrated in vacuo