Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 19001387 | HCID 19001387 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 19001374 | HCID 19001374 | 88.8% |
Reaction Steps
A mixture of the product of Step G (38 g, 0.087 mol) 200 mL of methanol, and 18 g (0.50 mol) hydrogen chloride was heated at reflux (66° C.) for 21/2 hours. The solution was concentrated, toluene (50 mL) was added to the residue and, the mixture concentrated again. Another 50 mL toluene was added and evaporated a second time. After adding 100 mL of toluene, the slurry was chilled, and then filtered. The solid was washed with toluene, then hexanes to yield 26 g of a pale yellow product, m.p. 175°-176° C., dec. Recrystallization from a mixture of tetrahydrofuran and methanol gave a colorless solid, m.p. 185°-186° C., dec.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05474998 |
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| Source dataset | uspto-grants-1995_12 |
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| ORD ID | ord-58014777c6834a819adde45cac4557fb |
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| Source note | uspto-grants-1995_12 |
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