Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Methylthio-2-imidazoline hydroiodide | HCID 88369 | — |
| Reactant | HCID 22632481 | HCID 22632481 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 22632472 | HCID 22632472 | — |
Reaction Steps
30 mg (0.073 mmol) of 4-(4-chlorobenzoyl)-1-[2-(4-piperidinyl)-ethyl]-1,3,4,5-tetrahydrobenzo[e][1,4]diazepin-2-on obtained in step 1 in Example 168 and 178 mg (0.73 mmol) of 2-methylthio-2-imidazoline were dissolved in 7 ml of methanol. 0.2 mg (1.4 mmol) of triethylamine was added to the obtained solution, and they were stirred at 70° C. overnight. The solvent was evaporated, and the obtained crude product was treated by the reversed phase high-performance liquid chromatography with silica gel chemically bonded with octadodecyl group as the filler and then eluted with a solvent mixture of water and acetonitrile containing 0.1% (V/V) of trifluoroacetic acid. Acetonitrile was evaporated. After the extraction with dichloromethane, the title compound was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06825191B2 |
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| Source dataset | uspto-grants-2004_11 |
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| ORD ID | ord-8d1581127fa34d82ac7adb02cd9c1554 |
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| Source note | uspto-grants-2004_11 |
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