Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Reactant | (3-Isopropoxy-4-methoxy-phenyl)-(1,2,3-trimethoxy-8,9-dihydro-7H-benzocyclohepten-5-yl)-methanone | HCID 68923389 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 15986324 | HCID 15986324 | 56.9% |
Reaction Steps
97 (0.07 g, 0.16 mmol) was dissolved in 10 mL of anhydrous CH2Cl2 under nitrogen at 0° C. Anhydrous AlCl3 (44 mg, 0.33 mmol) was added and the reaction mixture was stirred for 2 h at 0° C. Saturated NH4Cl (5 mL) was added and the organic phase was separated. The aqueous layer was extracted with CH2Cl2 (10 mL) and the combined organic phases were dried over Na2SO4, filtered, solvents evaporated under reduced pressure. The crude product was purified by column chromatography (30:70 EtOAc:Hexanes) to yield tan colored oil as product 24 (35 mg, 56% yield). Rf: 0.23 (60:40 Hex:EA).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08394859B2 |
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| Source dataset | uspto-grants-2013_03 |
|---|
| ORD ID | ord-d03624852d304c138678b600d67cb42b |
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| Source note | uspto-grants-2013_03 |
|---|
