HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 135869950, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | TBAF tetrahydrofuran | HCID 11078149 | — |
| Reactant | HCID 45280078 | HCID 45280078 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 135869950 | HCID 135869950 | 93.5% |
Reaction Steps
Tert-butyl6-(tert-butyldiphenylsilyloxy)-3-cyclopropylindazole-1-carboxylate (5.08 g) which can be prepared according to the method described in Reference example 6, etc. was dissolved in THF (53 mL; manufactured by Kanto Chemical Co., Inc.), and added with 1 mol/L-TBAF-THF solution (19.82 mL), followed by stirring at room temperature for 0.5 hours. To the reaction solution, water and brine were added and extraction was carried out three times with ethyl acetate. The organic layer was washed water and brine and dried over anhydrous sodium sulfate. After the solvent was evaporated under reduced pressure, the residue was purified by column chromatography (“COLUMN-B”; n-hexane:ethyl acetate=95:5→74:26) to obtain the title compound (2.54 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08304443B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-3488b7c2376044279d4ab229ac156a5c |
| Source note | uspto-grants-2012_11 |