Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | HCID 14851913 | HCID 14851913 | — |
| Reactant | HCID 14894666 | HCID 14894666 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 14851911 | HCID 14851911 | — |
Reaction Steps
The title compound was prepared by coupling (S)-6-(2-fluorophenyl)-8-iodo-4,1-dimethyl-4H[1,2,4]triazolo[4,3-a][4,1]benzodiazepine with 3,4-dihydro-1-(2-propynyl)-2(1H)-quinolinone under the conditions used in Example 100. The product was isolated by chromatography over the 50-fold amount of silica gel using 5% (v/v) of ethanol in methylene chloride for elution. The combined clean fractions were evaporated and the residue crystallized very slowly from ethanol/ether to give colorless crystals of (S)-1-{3-[6-(2-fluorophenyl)-4,1-dimethyl4H-[1,2,4]-triazolo[4,3-a][4,1]benzodiazepin-8-yl]-2-propynyl}3,4-dihydro-2(1H)-quinolinone with m.p. 155°-160° with foaming. These crystals contained both ethanol and water according analytical and spectral data. [α]D=+87.5° (c=1.0091 in CH2Cl2)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04959361 |
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| Source dataset | uspto-grants-1990_09 |
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| ORD ID | ord-569d0e72b9e5461eab378e2c9452b8a4 |
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| Source note | uspto-grants-1990_09 |
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