Triethylamine → 4-(1-{[3-Chloro-6-(trifluoromethyl)-1-benzothiophen-2-yl]carbonyl}azetidin-3-yl)-1-pyrimidin-2-ylpiperazin-2-one

関与物質

反応手順

A solution of intermediate 3c (prepared by procedures described in Example 4) in CH2Cl2 (2 mL) and TFA (0.5 mL) was stirred at room temperature for 1h. The solution was concentrated, and the residue was dissolved in CH2Cl2 (2.5 mL). To the resulting solution at 0° C. was added Et3N (0.11 mL, 0.79 mmol), followed by a solution of 3-chloro-6-trifluoromethyl-benzo[b]thiophene-2-carbonyl chloride 5a (prepared from 3-chloro-6-trifluoromethyl-benzo[b]thiophene-2-carboxylic acid following the procedures described in Example 1, Step A) (0.14 mmol) in CH2Cl2 (1.5 mL). The reaction was slowly warmed up to room temperature in 2 h, and was then quenched with aq. NaHCO3. The mixture was extracted with CH2Cl2. The organic solution was dried over Na2SO4 and concentrated. Purification by column chromatography (silica gel, 3% MeOH/CH2Cl2) gave Cpd 8 as yellow solid (28 mg). MS 496 (M+H+).

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