Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Formic Acid | HCID 284 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 178448837 | HCID 178448837 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 21562359 | HCID 21562359 | — |
Reaction Steps
A stirred solution of 0.02 mole of 7-chloro-3-methyl-5-phenyl-2-[(1-methyl-2-propynyl)amino]-3H-1,4benzodiazepine (IV), 20 ml. of acetic acid, 20 ml. of 88% formic acid and 1.5 ml of water at ambient temperature is treated, dropwise, with 160 ml. of a 5% aqueous solution of mercuric acetate. The mixture is then stirred at room temperature for about 3 hours, poured into ice water and then extracted with chloroform. The extract thus obtained is washed with water and then concentrated in vacuo. The residue thus obtained is suspended in hot ethyl acetate and filtered. The filtrate is concentrated and chromatographed on silica gel with 50% ethyl acetate-hexanes to give 8-chloro-6-phenyl-2,4-dimethyl-4H-imidazo[1,2-a][1,4]benzodiazepine-1-carboxaldehyde.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US03933794 |
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| Source dataset | uspto-grants-1976_01 |
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| ORD ID | ord-e297c97884c74ec09a6bbdb300443c35 |
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| Source note | uspto-grants-1976_01 |
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