HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → HCID 10605652, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Reactant | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| Reactant | HCID 10597882 | HCID 10597882 | — |
| Reactant | HCID 10814358 | HCID 10814358 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 10605652 | HCID 10605652 | 76.9% |
Reaction Steps
To a mixture of H-DTrp(2-CN)-DAsp(OMe)-OtBu (26 mg, prepared in Example (9-b)) and Boc-Pro-DPen(Me)-Leu-OH (33 mg, prepared in Example (9-f)) in DMF (3 mL) were added HOBT·H2O (12 mg) and EDCI·HCl (15 mg) under ice-cooling. The mixture was stirred under ice-cooling for 1 h and at room temperature for 1.5 h. The mixture was diluted with ethyl acetate (30 mL), washed with sat. aq. NaHCO3 (15 mL), 10% aq. citric acid (15 mL) and brine (15 mL) successively, dried over MgSO4 and evaporated under reduced pressure. The residue was purified by preparative TLC (Merck, Kieselgel 60 F254) with chloroform/methanol=30/1 for development to give the product (42 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05494897 |
| Source dataset | uspto-grants-1996_02 |
| ORD ID | ord-686d631f4fc740bd9762199abbcb1309 |
| Source note | uspto-grants-1996_02 |