HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 86754341, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | (S)-3-amino-2-benzenesulfonylamino-propionic acid tert-butyl ester hydrochloride | HCID 22853534 | — |
| Reactant | HCID 53849864 | HCID 53849864 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86754341 | HCID 86754341 | — |
Reaction Steps
A DMF solution (10 mL) containing 31-3 (301 mg, 1.0 mmol) 2-1 (336 mg, 1.0 mmol), HOBT (206 mg, 1.35 mmol), EDC (258 mg, 1.35 mmol) and NMM (440 μl, 4.0 mmol) was stirred under ambient conditions for 18 h. The DMF was evaporated and the residue partitioned between CH2Cl2 and H2O. The organic layer was dried (MgSO4) and concentrated to a yellow gum which was purified by flash chromatography (silica, 4:1, CHCl3 ·NH3 /IPA) to provide impure 31-4 which was rechromatographed (silica, 9:1 EtOAc/IPA) to give 31-4 as a colorless foam.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05929120 |
| Source dataset | uspto-grants-1999_07 |
| ORD ID | ord-b14848722f0d4399b5d7f3a79413d3ca |
| Source note | uspto-grants-1999_07 |