Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | HCID 69956107 | HCID 69956107 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane methanol | HCID 21226129 | — |
| Product | HCID 69954724 | HCID 69954724 | — |
Reaction Steps
0.6 g (1.22 mmmol) of the product of Example 28A and 30 ml of THF are introduced into a reactor. After solubilization, a solution of 0.135 g of KOH in 8 ml of water is added and the mixture is kept stirring for 3 h at 20-25° C. The mixture is neutralized with 0.1 N HCl to pH 6.8 and the THF is evaporated off at 50° C. under a vacuum of 20 rnm Hg. The residue is chromatographed, eluting with CH2Cl2 progressively enriched with methanol. The product obtained is crystallized from 10 ml of CH2Cl2 and the precipitate is filtered off. 0.25 g is obtained (Yld=42.7%). M.p.>275° C.—TLC (85/15 CH2Cl2/MeOH): Rf=0.35.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06239130B1 |
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| Source dataset | uspto-grants-2001_05 |
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| ORD ID | ord-78618c1aa24641c28410d2dd7159f590 |
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| Source note | uspto-grants-2001_05 |
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