HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 67209443, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | Acetic acid, 2-[(3-chloro-1,4-dimethyl-1H-pyrazolo[3,4-b]pyridin-6-yl)oxy]-, ethyl ester | HCID 67209453 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 67209443 | HCID 67209443 | — |
Reaction Steps
To a solution of Ethyl 2-((3-chloro-1,4-dimethyl-1H-pyrazolo[3,4-b]pyridin-6-yl)oxy)acetate in dioxane (5 ml) were added H2O (2.5 ml) and LiOH (111 mg, 4.65 mmol). After 2 h, more water was added and the mixture extracted with CH2Cl2. Then, the aqueous phase was acidified by drop wise addition of conc. HCl until the product precipitated. The title compound (580 mg, 98%) was filtered off and dried under reduced pressure. [1H-NMR (DMSO-d6, 400 MHz) δ 6.62 (s, 1H), 4.98 (s, 2H) 3.84 (s, 3H), 2.61 (s, 3H); HPLC-MS RtJ=0.81 min; [M+H]+=255.9, 258.0]
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08742106B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-801b04a656ff4087813d25b7027b884a |
| Source note | uspto-grants-2014_06 |