HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 85615690, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | Toluene methanol | HCID 21867641 | — |
| Reactant | HCID 85615714 | HCID 85615714 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 85615690 | HCID 85615690 | 75.5% |
Reaction Steps
To a solution of the ester (5 g, 12.16 mmole) of Step G, in dry tetrahydrofuran (66 mL) is added 1N-LiOH (37 mL, 37 mmole) and the mixture is stirred under nitrogen at room temperature for 2.5 hours (TLC, toluene-MeOH 9:1). The tetrahydrofuran is evaporated and the residue is diluted with water, acidified (to pH 6.5) with 10% acetic acid and extracted with ethyl acetate (3×). The extracts are washed with brine, dried (MgSO4) and evaporated to dryness. The crude product (4.94 g, pale yellow solid) is recrystallized from ethyl acetate to provide 3.65 g (75%) of the pure title compound (white solid, m.p. 146°-147° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05218124 |
| Source dataset | uspto-grants-1993_06 |
| ORD ID | ord-c1b01d6824a34f69a7295d37de9ed467 |
| Source note | uspto-grants-1993_06 |