Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 10225443 | HCID 10225443 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 9902690 | HCID 9902690 | 100% |
Reaction Steps
A solution of 4N hydrogenchloride in ethyl acetate (20 ml) was added to a solution of tert butyl 4-(2,2,4,6,7-pentamethyl-3-pyrrolidinyl-2,3-dihydro-1-benzofuran-5-yl)piperazinecarboxylate (3.55 g, 8 mmol) obtained in Example 132 in THF (20 mL) and ethyl acetate (20 ml) and the mixture was stirred at 60° C. for 3 hours. The resulting mixture was cooled to 0° C. made to weakly alkaline using 1N sodium hydroxide aqueous, and extracted with ethyl acetate. The organic extract was washed using saturated aqueous sodium chloride, dried over anhydrous sodium sulfate, and the solvent was removed under reduced pressure. The residue was purified with basic silica gel column chromatography (ethyl acetate) to obtain 2.72 g (yield 100%) of the title compound as an amorphous powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07208495B2 |
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| Source dataset | uspto-grants-2007_04 |
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| ORD ID | ord-26cc05fe3d6842038e782d4a8fd37965 |
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| Source note | uspto-grants-2007_04 |
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