HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 69540415, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | 4-Hydroxy-3,5-dimethylbenzoic acid | HCID 138387 | — |
| Reactant | HCID 22948699 | HCID 22948699 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 69540415 | HCID 69540415 | 62% |
Reaction Steps
To a solution of 13a and 3,5-dimethyl-4-hydroxybenzoic acid (307 mg, 1.85 mmol) in 5 ml each of DMF and CH2Cl2 was added HOBT (250 mg, 1.85 mmol), EDC (421 mg, 2.2 mmol), and triethylamine (0.64 ml, 4.56 mmol). The reaction was stirred at room temp. for 18 hrs. then diluted with EtOAc (150 ml) and washed with 10% NaHSO4, sat. NaHCO3 and sat. NaCl. The organic layer was dried over anhydrous Na2SO4, filtered, and evaporated in vacuo to afford a gum that was purified by flash chromatography eluting with CH2Cl2/EtOAc (7/3) to afford 545 mg (62%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06350741B1 |
| Source dataset | uspto-grants-2002_02 |
| ORD ID | ord-32c88bc2bd494a339a09138c8deda2b2 |
| Source note | uspto-grants-2002_02 |