HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-(Pyridin-3-yl)ethan-1-amine → HCID 178477861, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-(Pyridin-3-yl)ethan-1-amine | HCID 854051 | — |
| Reactant | 8-Chloro-5,10-dihydro-dibenzo[b,e][1,4]diazepin-11-thione | HCID 12535778 | — |
| Solvent | Glycol monoethyl ether | HCID 8076 | — |
| Product | HCID 178477861 | HCID 178477861 | 74% |
Reaction Steps
A solution of 0.5 g (1.9 mmol) of 8-chloro-5,10-dihydro-dibenzo[b,e][1,4]diazepin-11-thione in 10 mL of 2-ethoxyethanol was treated with 0.46 g (3.8 mmol) of 3-(2-aminoethyl)pyridine and heated at reflux overnight. The solvent was removed under reduced pressure and the residue taken up in EtOAc and washed five times with H2O, then saturated NaCl solution. Drying over MgSO4 and removal of the solvent under reduced pressure gave the crude product. Recrystallization from acetone/water gave 0.49 g (74% yield) of the product as a yellow solid, mp 195-196° C. The structure was confirmed by NMR and mass spectroscopy. (m+H)+ =349.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05919780 |
| Source dataset | uspto-grants-1999_07 |
| ORD ID | ord-8eddc349b20a45a78d2a012779a51de2 |
| Source note | uspto-grants-1999_07 |