Yield:350996-89-3 5%

Reaction Conditions:

with sulfur;diethylamine in ethanol at 20;

Steps:

48.a

Example 48 4-Ethyl-5-methyl-2-(2-(3-(trifluoromethyl)-4,5,6,7-tetrahvdroindazole-1-yl)acetamido) thiophene-3-carboxamidea) 2-Amino-4-ethyl-5-methylthiophene-3-carboxamide2-pentanone (1.52 g, 17.6 mmol), cyanoacetamide (1.50 g, 17.6 mmol) and sulphur (560 mg, 17.6mmol) were stirred in EtOH (6 ml_). Diethylamine (2 mL, 19.4 mmol) was added and the reaction stirred at RT overnight. Water (20 mL) was added and the precipitate filtered off and washed with heptane (100 mL) to give the product as a cream solid (150 mg, 0.81 mmol, 5 %).1 H NMR (400MHz, CDCI₃): δ 1.17 (t, 3H), 2.18 (s, 3H), 2.61 (q,2H), 5.48 (bs,2H), 5.84(bs, 2H).

References:

WO2008/3452,2008,A1 Location in patent:Page/Page column 47