反应详情

Prepared by analogy to Example 13 by reaction of 2-hydroxy-2-(2-trifluoromethyl-thiazol-4-yl)ethanamine with 1-(4-carbomethoxymethoxyphenyl)propan-2-one and sodium cyanoborohydride in methanol=(reaction time: 5 hours) followed by purification on a silica gel column using methylene chloride/methanol 20:1. This results in an approximately 50:50 diastereomer mixture of the base. This is recrystallised from a mixture of ether/ethyl acetate=65:10, and twice more from ethyl acetate. This results in diastereomer A in 98-99% purity.

1. customfollowed by purification on a silica gel column
2. customThis results in an approximately 50:50 diastereomer mixture of the base
3. customThis is recrystallised from a mixture of ether/ethyl acetate=65:10
4. customThis results in diastereomer A in 98-99% purity