ETHYL 2-ISOTHIOCYANATO-4,5-DIMETHYLTHIOPHENE-3-CARBOXYLATE synthesis
- Product Name:ETHYL 2-ISOTHIOCYANATO-4,5-DIMETHYLTHIOPHENE-3-CARBOXYLATE
- CAS Number:85716-85-4
- Molecular formula:C10H11NO2S2
- Molecular Weight:241.33
Yield:85716-85-4 100%
Reaction Conditions:
with calcium carbonate in chloroform;water at 0; for 3.5 h;
Steps:
50.b
To a mixture of thiophosgene (5.10 mL, 7.64 mmol) and calcium carbonate (1.05 g, 10.54 mmol) in CHCl3/H2O (1/2 by volume, 6 mL) was added dropwise a solution of ethyl 2-amino-4,5-dimethylthiophene-3-carboxylate (1.05 g, 5.27 mmol) in CHCl3 (7 mL) at 0° C. over a period of 1 h. The reaction mixture was the stirred for 2.5 h at 0° C., washed with water (3*). The organic layer was dried over MgSO4, filtered and concentrated to give the title compound (1.21 g, 100%). 1H NMR (400 MHz, DMSO-d6) δ 1.32 (t, 3H, J=7.1 Hz), 2.19 (s, 3H), 2.30 (s, 3H), 4.28 (q, 2H, J=7.1 Hz).
References:
US2008/306053,2008,A1 Location in patent:Page/Page column 67
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