HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 131732923, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | 4-tert-Butyl hydrogen N-((phenylmethoxy)carbonyl)-L-aspartate | HCID 111082 | — |
| Reactant | HCID 131732921 | HCID 131732921 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 131732923 | HCID 131732923 | 66.8% |
Reaction Steps
3-(1-naphtyl)-L-alanine-Val-OAllyl (0.394 g, 1.11 mmol) was solvated in CH2Cl2 (1.5 mL) and DMF (3 ml) followed addition of Z-Asp(OtBu)-OH (0.369 g, 1.03 eq), DMAP (14.8 mg, 0.11 eq) and 4-methylmorpholine (0.125 ml, 1.02 eq), then EDC (0.221 g, 1.04 eq). The vial was rinsed with 0.5 ml of dichloromethane. The mixture was stirred for 2 hours at room temperature. Then it was extracted using CH2Cl2/brine. The organic layer was dried over MgSO4, filtered off and concentrated. The obtained residue was purified on silica using a gradient EtOAc/Hex (0 to 80%) to get 0.516 g of the desired compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09045524B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-fdb71daeb41c4911b9b1c6ffb5f0ead9 |
| Source note | uspto-grants-2015_06 |