HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 24694245, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 60735499 | HCID 60735499 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 24694245 | HCID 24694245 | 98.2% |
Reaction Steps
To the solution of the ester 14 (0.43 g, 2.0 mmol) in THF (18 mL) was added LiOH.H2O (0.17 g, 4 mmol) as a solution in 5 mL of H2O. The reaction mixture was stirred at room temperature and monitored by TLC. When no staring material was observed, the reaction mixture was acidified with 1N HCl, (˜4.5 mL) and concentrated under reduce pressure to remove the organic solvent. The mixture was diluted with 15 mL of H2O and extracted with EtOAc (2×120 mL). The organic layer was washed with brine, dried over Na2SO4, concentrated and dried under high vacuum over P2O5 to give 0.40 g (98% yield) of compound 15 which was used in subsequent reaction without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07998980B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-83f7ed07a2d34ad4a55780fec6d6b5cd |
| Source note | uspto-grants-2011_08 |