HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Chloroaniline → HCID 9908998, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Chloroaniline | HCID 7932 | — |
| Reactant | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Reactant | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| Reactant | Ether hydrochloride | HCID 10953452 | — |
| Reactant | HCID 70298542 | HCID 70298542 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 9908998 | HCID 9908998 | — |
Reaction Steps
To a 0° C. solution of acid 6 (141 mg) in 2 mL of dry DMF was added triethylamine (0.089 mL), and 3-chloroaniline (0.046 mL). 1-Hydroxybenzotriazole hydrate (80 mg) was added, followed by 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (106 mg). After six hours, the reaction was poured into EtOAc, washed with sat. aq. NaHCO3 solution and brine, then dried (Na2SO4), filtered, and concentrated in vacuo to provide the crude product. Purification by silica gel chromatography (2-6% MeOH/CH2Cl2) gave a white foam which was taken up in CH2Cl2, treated with 1 M HCl/ether solution, and concentrated in vacuo. The product hydrochloride 1 was isolated as a white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05968965 |
| Source dataset | uspto-grants-1999_10 |
| ORD ID | ord-b4b5da662cdc4f8fb294c9369ce6395a |
| Source note | uspto-grants-1999_10 |