HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → HCID 59468917, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 59468927 | HCID 59468927 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 59468917 | HCID 59468917 | 97% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
To a solution of 1-(1,1-dimethylethyl) 2-methyl (2S,5R)-5-[4-{[(2-fluorophenyl)methyl]oxy}-3-(methyloxy)phenyl]-2-methyl-1,2-pyrrolidinedicarboxylate (D59, 160 mg, 0.34 mmol) in MeOH (1 ml) was added a solution of LiOH.H2O (29 mg, 0.68 mmol) in H2O (0.5 ml) and the mixture was heated in a microwave synthesizer for 70 min at 100° C. After evaporation of methanol, the aqueous phase was acidified to pH 3.5/4 with a solution of citric acid and extracted with ethyl acetate. The organic layer was dried (Na2SO4), filtered and evaporated affording the title compound (white solid, 150 mg, 97%); Rt (HPLC): 5.89 min. MS: (ES/−) m/z: 482 [M+Na] C25H30FNO6 requires 459.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08153623B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-987b3e6004ab4608a54cb4da4369fd6e |
| Source note | uspto-grants-2012_04 |