HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 21467116, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 14029304 | HCID 14029304 | — |
| Reactant | HCID 21467111 | HCID 21467111 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 21467116 | HCID 21467116 | — |
Reaction Steps
A 100 mL round bottom flask was charged with 3-amino-3,4-dihydro-1H-benzo[b]azepin-2,5-dione (4 g, 17.6 mmole), EDC (3.38 g, 17.6 mmole), HOBT (2.38 g, 17.6 mmole), 2,4-dichlorophenyl propionic acid (3.86 g, 17.6 mmole), Dimethylformamide (100 mL), and triethylamine (1.78 g, 17.6 mmole). The reaction mixture was stirred at room temperature for 1 hr. and then poured into saturated sodium bicarbonate (500 mL). The aqueous mixture was extracted with ethyl acetate (3×200 mL). The combined organics were dried over anhydrous magnesium sulfate, filtered, and concentrated at reduced pressure. The resulting solid was swished with a minimum of hot chloroform and filtered to give the product, 5.8 g (84%) mp 234°-236° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05696111 |
| Source dataset | uspto-grants-1997_12 |
| ORD ID | ord-0f206daf01b840d293da931e1ae962bd |
| Source note | uspto-grants-1997_12 |