Diisopropylethylamine → [5-(2-Chloro-6-methyl-pyridin-4-yl)-3-(2,2-difluoro-benzo[1,3]dioxol-5-ylamino)-[1,2,4]triazol-1-yl]acetic acid ethyl ester

Participants

Reaction Conditions

Reaction Steps

Intermediate D2 (13.6 g; 0.0340 mol), 2-hydrazinylacetic acid ethyl ester, hydrochloride (1:1) (10.5 g; 0.0680 mol), N-ethyl-N-(1-methylethyl)-2-propanamine (13.2 g; 0.1020 mol) and t-BuOH (400 ml) were refluxed for 2 hours. The reaction mixture was then evaporated. Water was added and the product was extracted with CH2Cl2. The organic layer was dried on MgSO4, filtered and evaporated in vacuo. The residue was then heated to 60° C. in ethanol/HCl for 1 hour. The reaction mixture was partly evaporated and, the precipitate was filtered off and dried. Yield: 4.57 g of intermediate D3.

Provenance & Evidence