Water → HCID 86670902, compound

Participants

Reaction Steps

To suspension of ethyl 7-amino-1-(tetrahydro-2H-pyran-4-yl)-1,4-dihydropyrazolo[3′,4′:4,5]thiopyrano[3,2-d][1,3]thiazole-3-carboxylate 5,5-dioxide (71 mg; 0.18 mmol; 1 eq.) and triethylamine (98.8 μL; 0.71 mmol; 4 eq.) in DCM (710 μL) at 0° C. is added acetylchloride (30 μL; 0.46 mmol; 2.5 eq.). The suspension is stirred at rt overnight then heated up to 100° C. for 1 day. Water is added to reacture mixture and the product is extracted with DCM (×2). The combined organic layers are washed with brine, dried over Na2SO4 then concentrated under vacuum affording a beige solid residue. The residue is triturated then sonicated in Et2O and the solid is filtered-off to afford the title compound. HPLC (max plot) 98.8%; Rt 3.28 min. MS (ESI+): 441.1.

Provenance & Evidence