反应详情

To a solution of 250 mg (0.91 mmol) of dimethyl malonate, malonate, 314 mg (2.72 mmol) of N-ethylmorpholine, 153 mg (1.0 mmol) of HOBt hydrate and 155 mg (1.0 mmol) of EDAC in 7 ml of DMF was added a solution of 202 mg (0.91 mmol) of 2-(3-tert-butylphenoxy)propionic acid in 3 ml of DMF. After 18 h at room temperature, the reaction mixture was concentrated completely 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 15 minutes 10% B→90% B). The product fractions were freeze-dried to give 323 mg (74%) of dimethyl 2-(1-{4-[2-(3-tert-butylphenoxy)propionylamino]phenyl}but-2-ynyl)malonate.

1. concentrationthe reaction mixture was concentrated completely
2. customseparated by means of preparative HPLC (Merck Hibar Purospher Star RP-18e 10 μm 25×250 mm
3. waitin 15 minutes 10% B→90% B)
4. customThe product fractions were freeze-dried