Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | Methanol tetrahydrofuran water | HCID 21892291 | — |
| Reactant | HCID 86653736 | HCID 86653736 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 67167837 | HCID 67167837 | 97.6% |
Reaction Steps
To a suspension of 0.87 g (2.1 mmol) of the compound obtained from step 2.4 in a 1/1/1 mixture of THF/methanol/water (12 ml) is added 0.134 g (3.2 mmol) of lithium hydroxide in a single portion. The reaction mixture is heated at 70° C. for 3 hours, and then cooled to room temperature. Water (10 ml) is added and the medium is acidified with HCl solution (1N) to pH 2, and the precipitate formed is isolated by filtration and dried over P2O5. 0.78 g of product is obtained in the form of a white powder. Yield=96%. Melting point 260° C. MH+: 381.1 (tr: 6.74 min., condition 1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08436011B2 |
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| Source dataset | uspto-grants-2013_05 |
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| ORD ID | ord-44221a44a7c449d3bb847e0780b3725d |
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| Source note | uspto-grants-2013_05 |
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