HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetamidine monohydrochloride → 6,7-dihydro-2-methyl-7-(4-nitrobenzoyl)-5H-pyrimido[5,4-d][l]benzazepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetamidine monohydrochloride | HCID 67170 | — |
| Reactant | 4-[(dimethylamino)methylene]-1,2,3,4-tetrahydro-1-(4-nitrobenzoyl)-5H-1-benzazepin-5-one | HCID 53653564 | — |
| Reactant | HCID 178418582 | HCID 178418582 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 6,7-dihydro-2-methyl-7-(4-nitrobenzoyl)-5H-pyrimido[5,4-d][l]benzazepine | HCID 54379793 | 99.7% |
Reaction Steps
To a stirred solution of 0.233 g of acetamidine hydrochloride in 36 ml of methyl alcohol under argon is added 0.133 g of NaOCH3. After 5 minutes, 0.600 g of 4-[(dimethylamino)methylene]-1,2,3,4-tetrahydro-1-(4-nitrobenzoyl)-5H-1-benzazepin-5-one is added and stirring continued for 18 hours. The volatiles are evaporated to a residue which is dissolved in ethyl acetate and passed through a pad of silica gel. The filtrate is evaporated in vacuo to is give 590 mg of the desired product as tan crystals, m.p. 211°-212° C. HR FABMS: Exact mass (M+H):361.1295.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05834461 |
| Source dataset | uspto-grants-1998_11 |
| ORD ID | ord-06be943289d54cc7b443c1db275ec851 |
| Source note | uspto-grants-1998_11 |