反应详情

In an alternative procedure, compound 8 (33.3 g, 0.12 mol) is added portionwise to a 0° C. commercially available solution of hydrogen chloride in 1,4-dioxan (Aldrich, 4 M, 750 ml.) Compound 8 slowly dissolves to afford a clear yellow solution. After stirring for approximately 30 minutes, the reaction mixture turns cloudy. The starting material is consumed in about two hours, as determined by TLC on silica using methylene chloride:ethyl acetate (9:1) as the eluent. The reaction mixture is filtered and a colorless solid product is obtained. The solid is washed exhaustively with ether (1L) to afford 19.2 g (76%) of compound 9.

1. dissolutionslowly dissolves
2. customto afford a clear yellow solution
3. customThe starting material is consumed in about two hours
4. filtrationThe reaction mixture is filtered
5. customa colorless solid product is obtained
6. washThe solid is washed exhaustively with ether (1L)