HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 59456957, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | N,N-Dimethylethylenediamine | HCID 66053 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | 2-Amino-5-bromopyridine-3-carboxylic acid--hydrogen bromide (1/1) | HCID 57350554 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59456957 | HCID 59456957 | 70% |
Reaction Steps
To a suspension of 2-amino-5-bromo-nicotinic acid hydrobromide (4.00 g, 13.4 mmol) in CH2Cl2 (150 mL) was added Et3N (2.79 mL, 20.1 mmol), EDC (2.70 g, 14.1 mmol), and HOBt (1.91 g, 14.1 mmol) at 0° C., and the mixture was stirred for 10 min. N,N-dimethylethylenediamine was then added, and the mixture was allowed to stir overnight at room temperature. The organic solution was washed with 2 N NaOH (2×20 mL), H2O (2×20 mL) and brine, dried over Na2SO4 and filtered. The solvent was concentrated to give the title compound (2.70 g, 70%) as a yellow solid: MS (ESI) m/e 287 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07879872B2 |
| Source dataset | uspto-grants-2011_02 |
| ORD ID | ord-9205fb02785449789729b4fae9ab0f65 |
| Source note | uspto-grants-2011_02 |