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3-IsoxazolecarboxaMide, 5-[5-chloro-2,4-bis(phenylMethoxy)phenyl]-N-ethyl- synthesis
- Product Name:3-IsoxazolecarboxaMide, 5-[5-chloro-2,4-bis(phenylMethoxy)phenyl]-N-ethyl-
- CAS Number:747413-05-4
- Molecular formula:C26H23ClN2O4
- Molecular Weight:462.92
Yield:747413-05-4 93%
Reaction Conditions:
in ethanol at 80; for 5 h;
Steps:
1g Step 1g: 5-(2,4-Bis(benzyloxy)-5-chlorophenyl)-N-ethylisoxazole-3-carboxamide (Compound 0107)
Step 1g: 5-(2,4-Bis(benzyloxy)-5-chlorophenyl)-N-ethylisoxazole-3-carboxamide (Compound 0107) To a flask containing 0106 (4.40 g, 9.51 mmol) was added a solution of ethylamine in ethanol (2.0 M, 40 ml, 80 mmol). The mixture was heated to 80° C. and stirred for 5 h. The mixture was allowed to cool to ice-bath temperature, filtered and the solid was washed with cold ethanol, dried in vacuo to obtain 0107 as a white solid (4.10 g, 93%): LCMS: 463 [M+1]+. 1H NMR (CDCl3): δ 1.28 (t, J=6 Hz, 3H), 3.44-3.53 (m, 2H), 5.10 (s, 2H), 5.16 (s, 2H), 6.59 (s, 1H), 6.81 (t, J=6 Hz, 1H), 7.08 (s, 1H), 7.25-7.40 (m, 10H), 7.97 (s, 1H).
References:
US2009/76006,2009,A1 Location in patent:Page/Page column 28; 35