関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1895-39-2 | HCID 45051942 | — |
| 反応物 | Tert-butyl 6-(benzyloxy)-3-oxo-2,3-dihydroindazole-1-carboxylate | HCID 59370717 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | tert-Butyl 6-(benzyloxy)-3-difluoromethoxyindazole-1-carboxylate | HCID 45280135 | 67.5% |
反応手順
Tert-butyl 6-(benzyloxy)-3-oxo-2,3-dihydroindazole-1-carboxylate (342 mg) which can be prepared according to the method described in Reference example 32, etc. and potassium carbonate (2.0887 g; manufactured by Sigma-Aldrich Co.) were suspended in dehydrated DMF (10 mL; manufactured by Kanto Chemical Co., Inc.), added with sodium chlorodifluoroacetic acid (853 mg; manufactured by Tokyo Chemical Industry, Co., Ltd.), and stirred at 80° C. for 12 hours. The reaction solution was added to water and extraction was carried out twice with ethyl acetate. The organic layer was washed twice with water and once with brine and dried over sodium sulfate. After the solvent was evaporated under reduced pressure, the residue was purified by column chromatography (“COLUMN-A”; n-hexane:ethyl acetate=100:0→87:13) to obtain the title compound (264.7 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08304443B2 |
|---|
| 出典データセット | uspto-grants-2012_11 |
|---|
| ORD ID | ord-4cfb48990f0746ec86dce3827fff5c7c |
|---|
| 出典メモ | uspto-grants-2012_11 |
|---|