4-Methylmorpholine → HCID 53495945, 화합물

참여 물질

반응 단계

(R/S)-2-Hydroxy-2-(4-(5-(5-phenyl-4-(trifluoromethyl)isoxazol-3-yl)-1,2,4-oxadiazol-3-yl)phenyl)acetic acid (Int-IX, 30 mg, 0.070 mmol), 2-amino-N-methylacetamide (9.19 mg, 0.104 mmol), HATU (34.4 mg, 0.090 mmol), and 4-methylmorpholine (70.4 mg, 0.696 mmol) were added to DMF (1 mL). This was stirred overnight before it was purified by prep HPLC (PHENOMENEX® Luna 5u 21×250 mm, gradient elution with Method 1—MeOH/water containing 0.1% trifluoroacetic acid as defined above, 0% B to 100% B over 30 min, 25 mL/min, 220 nM, product retention=29.0 min) to provide (R/S)-2-hydroxy-N-(2-(methylamino)-2-oxoethyl)-2-(4-(5-(5-phenyl-4-(trifluoromethyl)isoxazol-3-yl)-1,2,4-oxadiazol-3-yl)phenyl)acetamide (3.5 mg, 6.28 μmol, 9.03% yield): LCMS=502.2 [M+H]+; 1H NMR (400 MHz, methanol-d4) δ ppm 8.55 (1 H, br. s.), 8.17 (2 H, d, J=8.14 Hz), 7.59-7.85 (7 H, m), 5.20 (1 H, s), 3.78-4.01 (2 H, m), 2.75 (3 H, s); HPLC peak RT=8.2 min (Method A).

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