Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 11681730 | HCID 11681730 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | HCID 11695645 | HCID 11695645 | — |
Reaction Steps
A mixture of Example 6 in ethanol (8 mL) and 1N NaOH (2.0 mL) was stirred at reflux for 1 hour and cooled to room temperature. The solution was acidified with 1N HCl (2.1 mL) and partially concentrated. The precipitated solid was collected by filtration, washed with water, dissolved in methanol, and filtered. The filtrate was concentrated by boiling to about 0.4 mL, and diluted with diethyl ether. The resulting precipitate was collected by filtration to provide the desired product as a colorless solid. ESI-MS, both positive and negative ion consistent for MW 331, 1H NMR (500 MHz, CD3OD) δ 1.42 (m, 3H), 1.86 (m, 7H), 3.14 (m, J=12.05, 12.05 Hz, 1H), 5.01 (s, 2H), 7.21 (t, J=7.48 Hz, 1H), 7.32 (t, J=7.48 Hz, 1H), 7.44 (d, J=7.63 Hz, 1H), 7.58 (s, 2H), 7.73 (d, J=7.63 Hz, 1H), 7.89 (s, 1H), 7.89 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07348425B2 |
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| Source dataset | uspto-grants-2008_03 |
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| ORD ID | ord-7291f74eb55a42dbad2f3d841b4ff430 |
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| Source note | uspto-grants-2008_03 |
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