反应详情

The operation is carried out as in Stage 2 of Example 5 starting from 160 mg of the product obtained in Stage 1 of Example 5, 3 ml of butanol and using 100 mg of ethyl 4-aminobenzoate in place of the benzylamine and the reaction medium is taken to a temperature of approximately 80 to 85° C. for 30 hours, left to return to ambient temperature, diluted with 3 ml of isopropanol, placed for approximately one hour at a temperature of approximately 0° C., followed by separating, washing with 5 ml of isopropanol and drying under vacuum at a temperature of approximately 50° C. After purification on silica eluting with methylene chloride/ethyl acetate in a proportion of 90/10, 202 mg of expected product is thus obtained in the form of white-cream crystals.

1. waitleft
2. customto return to ambient temperature
3. waitplaced for approximately one hour at a temperature of approximately 0° C.
4. customby separating
5. washwashing with 5 ml of isopropanol
6. customdrying under vacuum at a temperature of approximately 50° C
7. customAfter purification on silica eluting with methylene chloride/ethyl acetate in a proportion of 90/10, 202 mg of expected product
8. customis thus obtained in the form of white-cream crystals