HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 77442752, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Nicotinic Acid | HCID 938 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | HCID 86762483 | HCID 86762483 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 77442752 | HCID 77442752 | — |
Reaction Steps
A 100 mL round bottom flask was charged with a magnetic stirbar, EDC (3.8 g, 19.9 mmol), HOBT (4.1 g, 26.5 mmol), 5-methyl, 3-pyridine carboxylic acid (2.2 g, 15.9 mmol) and methylenechloride (35 mL). tert-Butyl 4-(aminomethyl)hexahydrocyclopenta[b]pyrrole-1(2H)-carboxylate (cis-isomer, racemic, >95% of one diastereomer, 3 g, 13.3 mmol) was added over 10 minutes and the reaction mixture was allowed to stir for 9 h at room temperature. The solvent was removed in vacuo, and the product was dissolved in chloroform and washed with water. The organic layer was dried with magnesium sulfate and solvent was removed in vacuo. The final compound was purified using reverse-phase HPLC to afford Compound 12. LC-MS, M+1=346.0
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08759539B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-0a0c7c4e3393483388141dc348c5c9d9 |
| Source note | uspto-grants-2014_06 |