Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | HCID 20321555 | HCID 20321555 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 20321574 | HCID 20321574 | — |
Reaction Steps
A solution of 0.33 g of 3-[4-chloro-2-(2-fluoro-benzoyl)-phenyl]-4-phthalimidomethyl-2-methyl-pyrazole in 20 ml of methanol is saturated with ammonia and allowed to stand at room temperature for 2 days. The residue obtained after removal of solvent is treated with water and then extracted with diethyl ether. The ether extract is washed with a diluted aqueous sodium hydroxide solution, water and a saturated solution of sodium chloride in water and dried over sodium sulfate. Removal of ether yields an oil which is then chromatographed on a column of silica gel, the material being eluted with ethyl acetate. The solid residue obtained after removal of ethyl acetate is crystallized from a mixture of ethyl acetate and petroleum ether to yield the 8-chloro-6-(2-fluorophenyl)-1-methyl-1H,4H-pyrazolo [4,3-d](2) benzazepine m.p. 127°-129°, which is identical with the compound prepared according to the process of example 2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04022801 |
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| Source dataset | uspto-grants-1977_05 |
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| ORD ID | ord-6b0ae4a0161f48ac8811918f6b53b9b0 |
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| Source note | uspto-grants-1977_05 |
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