Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | HCID 117831357 | HCID 117831357 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 117830931 | HCID 117830931 | — |
Reaction Steps
To a solution of 7.80 g (16.51 mmol) of the compound obtained in Step C in 100 mL of DMSO there are added 1.16 g (19.83 mmol) of solid sodium chloride (NaCl) and then, dropwise, 5 mL of water. The batch is stirred at 130° C. for 1 hour and then the solution is concentrated to 3/4. The reaction mixture is then diluted with dichloromethane and washed successively with saturated aqueous lithium chloride solution and then with brine. The organic phase is then dried over MgSO4, filtered and concentrated to dryness. After purification by chromatography over silica gel using cyclohexane and ethyl acetate as eluants, the expected product is obtained in the form of an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09108983B2 |
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| Source dataset | uspto-grants-2015_08 |
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| ORD ID | ord-c585954a317548588a4b9d82df534e5e |
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| Source note | uspto-grants-2015_08 |
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