HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → HCID 57988391, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 57988353 | HCID 57988353 | — |
| Solvent | Methanol tetrahydrofuran water | HCID 21892291 | — |
| Product | HCID 57988391 | HCID 57988391 | 88.7% |
Reaction Steps
The crude (1R,2S)-ethyl 1-(6-(3-chlorophenoxy)-2-((S)-2-(4-fluorophenylamino)-3,3-dimethylbutanoyl)-1,2,3,4-tetrahydroisoquinoline-3-carboxamido)-2-vinylcyclopropanecarboxylate (130 mg, 0.20 mmol) was dissolved in 1.0 mL of a mixture of THF:MeOH:H2O (2:1:1). Lithium hydroxide monohydrate (0.050 g, 1.2 mmol) was added and reaction stirred at rt overnight. The reaction was then concentrated under vacuum and quenched with 5 mL of 1 N HCl. The product precipitated and could be filtered off giving an off-white powder (110 mg). It was directly used in the next step without further purification. MS m/e 619 (M−−H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07932277B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-02e6f5f5d347433499cbb063f8500e54 |
| Source note | uspto-grants-2011_04 |