HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → HCID 68283607, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 68284416 | HCID 68284416 | — |
| Solvent | Methanol tetrahydrofuran water | HCID 21892291 | — |
| Product | HCID 68283607 | HCID 68283607 | — |
Reaction Steps
To 3-[({(2S,4R)-1-[2-(3-acetyl-indol-1-yl)-acetyl]-4-fluoro-pyrrolidine-2-carbonyl}-amino)-methyl]-5-chloro-4-fluoro-benzoic acid methyl ester Example 523 (35.0 mg, 0.066 mmol) in THF-MeOH—H2O (ratio 2:1:1; 1 mL) was added LiOH.H2O (2.76 mg, 0.066 mmol). The reaction mixture was stirred at RT for 4 h. Volatiles were evaporated and the residue was taken up in water, Acidification to pH=1 by addition of a 6M HCl solution formed a precipitate which was filtered and dried at 50° C. in vacuo for 1 h to afford the title compound as a solid. MS: 518.0 [M+H]+; tR (HPLC conditions c): 4.26 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09085555B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-adfefb762d4d45e3bee0731d30b29bc2 |
| Source note | uspto-grants-2015_07 |