참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Tributyltin Chloride | HCID 15096 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | HCID 178418918 | HCID 178418918 | — |
| 반응물 | HCID 178455421 | HCID 178455421 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 178448228 | HCID 178448228 | — |
반응 단계
In a round-bottomed flask, 7-(tert-butyl-dimethyl-silanyloxymethyl)-3-iodo-1H-indazole (200 mg, 0.52 mmol) was dissolved in THF (2.8 ml) and sodium hydride (60% in mineral oil, 25 mg, 0.63 mmol) was added. The reaction mixture was stirred at room temperature for 10 min then cooled to −16° C. (NaCl/ice bath) and isopropylmagnesium chloride (2.0 M in THF, 0.36 ml, 0.72 mmol) was added dropwise. The reaction mixture was stirred at −16° C. for 30 min then tributylchlorostannane (0.16 ml, 0.59 mmol) was slowly added. The reaction mixture was allowed to warm to room temperature and stirred for 2.5 h then quenched with saturated aqueous NH4Cl and extracted with EtOAc (2×). The organic layers were washed with water and brine then dried over sodium sulfate, filtered and concentrated to give 7-(tert-butyl-dimethyl-silanyloxymethyl)-3-tributylstannanyl-1H-indazole as a yellow oil which was used without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08658646B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_02 |
|---|
| ORD ID | ord-c4a28bd461a2440f83bc7b2096cfb94c |
|---|
| 출처 메모 | uspto-grants-2014_02 |
|---|