Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Dipyridodiazepinone deriv. 41 | HCID 463561 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 15956286 | HCID 15956286 | 15.9% |
Reaction Steps
Sodium hydride (0.013 g, 60% in oil) was added to a solution of 5,11-dihydro-11-ethyl-5-methyl-2-(2-pyrrolyl)-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (0.100 g) in dry DMF (3 mL) and stirred for 30 min. After cooling to 0° C., acetyl chloride (0.025 g) was added and the reaction mixture was allowed to warm to room temperature overnight. Water was added and the product was extracted with CH2Cl2, dried (anhyd Na2SO4), filtered, and evaporated. The residue was purified by preparative plate chromatography (ethyl acetate/hexanes, 1:1). Crystallization from ethyl acetate/pet ether gave 0.018 g of the title compound, mp 106°-108° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05837704 |
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| Source dataset | uspto-grants-1998_11 |
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| ORD ID | ord-9692b0225cea4f658c06c6575ef6eefb |
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| Source note | uspto-grants-1998_11 |
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