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 (3x). 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 | US05364944 |
| Source dataset | uspto-grants-1994_11 |
| ORD ID | ord-0d881ee76ba74d1faf48af4ff9c4901b |
| Source note | uspto-grants-1994_11 |