反应详情

A solution of 304 mg (0.67 mmol) of 2-(1-{4-[2-(3-tert-butylphenoxy)propionylamino]-phenyl}but-2-ynyl)malonic acid in 10 ml of dioxane was boiled at 120° C. for 27 h. The reaction mixture was concentrated and separated by means of preparative HPLC (Merck Hibar Purospher Star RP-18e 10 μm 25×250 mm; A: H2O+0.05% TFA; B: ACN+0.05% TFA; flow rate: 50 ml/min; in 10 minutes 10% B→80% B; in 5 minutes 80% B→90% B). The product fractions were freeze-dried to obtain 214 mg (78%) of 3-{4-[2-(3-tert-butylphenoxy)propionylamino]phenyl}hex-4-ynoic acid. C25H29NO4 (407.51), LCMS (ESI-pos): 408 (M+H+).

1. customfor 27 h
2. concentrationThe reaction mixture was concentrated
3. customseparated by means of preparative HPLC (Merck Hibar Purospher Star RP-18e 10 μm 25×250 mm
4. waitin 5 minutes 80% B→90% B)
5. customThe product fractions were freeze-dried