Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Lithium Chloride | HCID 433294 | — |
| Reactant | HCID 25023595 | HCID 25023595 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59397235 | HCID 59397235 | — |
Reaction Steps
To a solution of 2-benzyl-9a-(2-fluoroethyl)-8,9,9a,10-tetrahydroindeno[2,1-e]indazol-7(2H)-one (1.0 g, 2.5 mmol) in 25 mL, of dimethylformamide was added lithium chloride (1.05 g, 25 mmol) and the stirred mixture was heated to 150° C. After heating for 89 hours, the reaction mixture was cooled to room temperature and partitioned between EtOAc and water. The organic phase was washed thoroughly with water (3×) followed by brine and dried over MgSO4. The solution was concentrated under vacuum and the residue chromatographed on silica gel (elution with 15:85 to 75:25 EtOAc/hexanes) to yield 2-benzyl-2,9,10,11-tetrahydro-8,10a-methanoazuleno[2,1-e]indazol-7(8H)-one as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07923568B2 |
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| Source dataset | uspto-grants-2011_04 |
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| ORD ID | ord-24ff5347bcb4493386095284c40c07f2 |
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| Source note | uspto-grants-2011_04 |
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