HCID 69234263, compound → HCID 59843068, compound

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Reaction Steps

A solution of tert-butyl methyl(2-(3-(4-methylthiophen-2-yl)-6-oxopyridazin-1(6H)-yl)ethyl)carbamate (340 mg, 973 μmol) in CH2Cl2 (5 mL) and TFA (5 mL) was stirred for 30 min at 23° C. The solvents were removed under reduced pressure and the residue partitioned between CH2Cl2 (20 mL) and 1M NaOH (10 mL). The organic layer was dried over MgSO4, concentrated and purified on silica (12 g) eluting with 0-6% (2M NH3 in MeOH/CH2Cl2) to give the product as an amber oil. MS (ESI pos. ion) m/z (MH+): 250. Calc'd exact mass for C12H15N3OS: 249. 1H NMR (400 MHz, Chloroform-d) δ ppm 1.60 (br. s., 2 H) 2.28 (d, J=0.78 Hz, 3 H) 2.49 (s, 3 H) 3.07 (t, J=6.06 Hz, 2 H) 4.32 (t, J=6.06 Hz, 2 H) 6.88-7.01 (m, 2 H) 7.18 (d, J=1.17 Hz, 1 H) 7.54 (d, J=9.59 Hz, 1 H).

Provenance & Evidence