Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Imidazole | HCID 795 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | tert-Butyldiphenylchlorosilane | HCID 94078 | — |
| Reactant | 6-hydroxy-1H-indazole | HCID 135483987 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 59370713 | HCID 59370713 | — |
Reaction Steps
Indazol-6-ol (4.029 g) which can be prepared according to the method described in Reference example 35, etc. was dissolved dehydrated DMF (60 mL; manufactured by Kanto Chemical Co., Inc.), and added with imidazole (4.49 g; manufactured by Tokyo Chemical Industry, Co., Ltd.) and TBDPSCl (17.1 mL; manufactured by Tokyo Chemical Industry, Co., Ltd.). The mixture was stirred overnight at room temperature. The reaction solution was added to water and extraction was carried out three times with ethyl acetate. The organic layer was washed three times with water and dried over anhydrous magnesium sulfate. After the solvent was evaporated under reduced pressure, the residue was purified by column chromatography (“COLUMN-A”; n-hexane:ethyl acetate=92:8→71:29) to obtain the title compound (9.214 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08304443B2 |
|---|
| Source dataset | uspto-grants-2012_11 |
|---|
| ORD ID | ord-2f1cebb63a504e058f3f088123477351 |
|---|
| Source note | uspto-grants-2012_11 |
|---|