HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 58413049, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | N-Hydroxysuccinimide | HCID 80170 | — |
| Reactant | HCID 58413177 | HCID 58413177 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 58413049 | HCID 58413049 | — |
Reaction Steps
EDC (290 mg) was added into a solution of 4-[2-((S)-1-tert-butoxycarbonyl-piperidin-3-yloxy)-4-fluoro-phenylamino]-5-methyl-thieno[2,3-d]pyrimidine-6-carboxylic acid (640 mg) and N-hydroxysuccinimide (218 mg) in anhydrous DMF (10 ml). The reaction was stirred at room temperature overnight. A further aliqout of EDC (58 mg) and N-hydroxysuccinimide (44 mg) were added and the reaction stirred for further 2 h. The DMF was removed in vacuo and the residue co-evaporated from toluene. The solid was portioned between EtOAc and water. The organic layer was separated and washed with brine. The combined organics were passed through a phase separator and concentrated in vacuo.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08648068B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-5a67e15cbd964e55b3274c533a15cb3c |
| Source note | uspto-grants-2014_02 |