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CAS No. : | 35212-90-9 | MDL No. : | MFCD02647200 |
Formula : | C10H8N2O4S | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 252.25 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Class: | ||
Precautionary Statements: | UN#: | ||
Hazard Statements: | Packing Group: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
36% | at 190.0℃; for 5.0h;Heating / reflux; Neat liquid(s); | A mixture of <strong>[35212-90-9]methyl 3-amino-6-nitrobenzothiophene-2-carboxylate</strong> (20 mg, 0.08 mmol) and formamidine acetate (59 mg, 0.57 mmol) was heated at 190 C. for 5 hours and cooled to 25 C. The reaction residue was triturated with water, and 7-nitrobenzo[b]thieno[3,2-d]-3H-pyrimid-4-one (7 mg, 36%) was obtained by Buchner filtration as a dark brown solid, mp >320 C. 1H NMR (DMSO-d6): delta 9.21 (d, J=1.7 Hz, 1H), 8.39 (d, J=8.5 Hz, 1H), 8.38 (s, 1H), 8.32 (dd, J 8.8, 2.0 Hz, 1H). Mass Spectrum (CI): 248 (100, MH+), 247 (30, M+). Analysis calculated for C1OH5N3O3S: C, 48.58; H, 2.04; N, 17.00%. Found: C, 48.19; H, 2.09; N, 16.77%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
54% | With triethylamine; In acetonitrile; at 25℃; for 19.0h; | Methyl 3-amino-6-nitrobenzothiophene-2-carboxylate: Methyl thioglycolate (0.08 mL, 0.85 mmol) was added to a solution of <strong>[34667-88-4]2-fluoro-4-nitrobenzonitrile</strong> (145 mg, 0.87 mmol), and triethylamine (0.14 mL, 1.0 mmol) in acetonitrile (20 mL) stirred under nitrogen at 25° C. After 3 hours further triethylamine (0.28 mL, 2.0 mmol) was added to the solution, which was stirred at 25° C. for a further 16 hours. The solvent was removed under reduced pressure to give a brown residue, which upon trituration with chloroform precipitated methyl 3-amino-6-nitrobenzothiophene-2-carboxylate (103 mg, 54percent) as a red brown solid, mp 228.5-229.5° C. 1H NMR (DMSO-d6): delta 8.87 (d, J=2.0 Hz, 1H), 8.32 (d, J=9.0 Hz, 1H), 8.15 (dd, J=8.8, 2.0 Hz, 1H), 7.26 (brs, 2H), 3.77 (s, 3H). Mass Spectrum (CI): 253 (100, MH+), 252 (52, M+). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
46% | In ethanol; | EXAMPLE 47C 3-Amino-2-carbomethoxy-6-nitro-benzthiophene The product from Example 47B (3.73 g, 19.3 mmol) was treated with 1 equivalent ethyl thioglycolate and 1 equivalent K2 CO3 in ethanol by the procedure described in Example 41A to yield the title compound (2.35 g, 46%). m.p. 169-170 C. 1 H NMR (300 MHz, DMSO) delta8.90 (d, 1H), 8.37 (d, 1H), 8.20 (dd, 1H), 7.29 (br s, 2H), 4.31 (q, 2H), 1.31 (t, 3H). MS (DCI/NH3) m/e 284 (M+NH4)+. |