Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Reactant | 3-Amino-5-(4-bromophenyl)thiophene-2-carboxylic acid | HCID 53443455 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 68504957 | HCID 68504957 | 44% |
Reaction Steps
3-amino-5-(4-bromophenyl)thiophene-2-carboxylic acid (11.21 mmol), N-methyl piperazine (11.21 mmol) and N-methylpyrrolidinone (13.5 mL) were mixed together The reaction mixture was stirred at 160° C. for 5 hours and cooled down to room temperature. EtOAc and water were added, organics were separated, dried over Na2SO4, concentrated under reduced pressure and filtrated over silica (DCM/MeOH). Diisopropyl ether was added to the crude material and the residue obtained was filtered to give Intermediate IX.1 as a beige solid in 44% yield, which was characterized by the following spectroscopic data: MS (ESI, EI+) m/z=255 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08193372B2 |
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| Source dataset | uspto-grants-2012_06 |
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| ORD ID | ord-f5faa2ebe2b840d1a9f5e818eefa61b3 |
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| Source note | uspto-grants-2012_06 |
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