HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 59497234, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 67377783 | HCID 67377783 | — |
| Solvent | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| Product | HCID 59497234 | HCID 59497234 | 100% |
Reaction Steps
3-[3-(4-Amino-3-tri fluoromethoxy-benzyl)-2-oxo-2,3-dihydro-benzimidazol-1-yl]-hexanoic acid ethyl ester—20 mg (0.04 mmol) is dissolved in 1.5 mL of dioxane/water (1:1) and then lithium hydroxide (4.1 mg, 0.17 mmol) is added. The reaction is stirred at room temperature and monitord by LC/MS. Upon completion the reaction is acidified by the addition of 1N HCl. The solvent is evaporated and the residue partitioned between ethyl acetate (2 mL) and water (2 mL). The organic layer is dried over anhydrous sodium sulfate. The solvent is evaporated and the resulting solid is purified by Combi flash chromatography, eluting with 0-20% methanol/dichloromethane to give the title compound (18 mg, 0.04 mmol 95%). LCMS (ESMS): m/z 438.4 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09150556B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-863a9871c52b4c5984b1ded1b37dbcf3 |
| Source note | uspto-grants-2015_10 |