HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methylmorpholine → 2'-Chloro-5'-[4-(4-methanesulfonyl-piperazin-1-ylmethyl)-phenylcarbamoyl]-biphenyl-4-carboxylic acid ethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | 4-(4-Methanesulfonyl-piperazin-1-ylmethyl)-phenylamine | HCID 11369231 | — |
| Reactant | 4-Chloro-3-(4-ethoxycarbonylphenyl)benzoic acid | HCID 53227884 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 2'-Chloro-5'-[4-(4-methanesulfonyl-piperazin-1-ylmethyl)-phenylcarbamoyl]-biphenyl-4-carboxylic acid ethyl ester | HCID 67372382 | 86.5% |
Reaction Steps
A mixture of 6-chloro-biphenyl-3,4′-dicarboxylic acid 4′-ethyl ester (152 mg), 4-(4-methanesulfonyl-piperazin-1-ylmethyl)-phenylamine (175 mg), EDAC (125 mg), HOBT (88 mg) and N-methylmorpholine (143 μl) in DMF (3 ml) was stirred at room temperature. After 1 h, water (30 ml) was added and the resulting suspension filtered. The residue was then purified by chromatography. Gradient elution with 30-100% ethyl acetate in petrol gave a beige solid (240 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08008303B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-2c822a64b725487aa99b53d73ee62db1 |
| Source note | uspto-grants-2011_08 |