HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 13376557, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Triethyl orthoacetate | HCID 66221 | — |
| Reactant | HCID 13376543 | HCID 13376543 | — |
| Product | HCID 13376557 | HCID 13376557 | 60% |
Reaction Steps
To a solution of 3.5 g (0.0154 m) of 1-[(2-aminophenyl)methyl]-2-methyl-1-phenylhydrazine of Example 9c in 40 ml of acetonitrile and 4.87 g (0.03 m) of triethyl orthoacetate was added sufficient ethereal HCl to make the solution acidic. The mixture was refluxed 5.5 hours. The solvents were evaporated and the residue was partitioned between 10% NaOH and ether. The ether extract was washed with water, dried (Na2SO4) and filtered. The product was precipitated with ethereal HCl to afford 2.63 g (60%) of 4,5-dihydro-2,3-dimethyl-4-phenyl-3H-1,3,4-benzotriazepine hydrochloride, m.p. 274°-277° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04482547 |
| Source dataset | uspto-grants-1984_11 |
| ORD ID | ord-965dc505e0334f6c96e443e8c373d6d0 |
| Source note | uspto-grants-1984_11 |