HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 58100944, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | HCID 66850507 | HCID 66850507 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 58100944 | HCID 58100944 | 80.3% |
Reaction Steps
0.23 g (4.06 mmol) of potassium hydroxide is added to a solution of 0.5 g (1.35 mmol) of ethyl 7-trimethylsilyl-1-[(3-fluorophenyl)methyl]-1H-indole-2-carboxylate, obtained according to the protocol described in stage 5.2, in 30 ml of a mixture (v/v/v) of methanol, water and dioxane. After stirring at reflux for three hours, the reaction mixture is one-third concentrated under reduced pressure and then taken up in 10 ml of water. The medium is acidified at pH 1 by successive additions of 1N hydrochloric acid. The precipitate is recovered by filtration, washed with water and then dried under reduced pressure. 0.37 g of the expected product is thus isolated, which product is used as it is in the subsequent stage.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08399491B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-c838337d24d349a79e9dc2b4c19173c0 |
| Source note | uspto-grants-2013_03 |