Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethyl Acetate → 2-(2-Trimethylsilanyl-ethoxymethyl)-2H-indazole-5-carbaldehyde
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | 2-Chloromethyl 2-(trimethylsilyl)ethyl ether | HCID 2724271 | — |
| 반응물 | alpha-Cyclohexylcyclohexanemethanamine | HCID 10774245 | — |
| 반응물 | HCID 178519387 | HCID 178519387 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-(2-Trimethylsilanyl-ethoxymethyl)-2H-indazole-5-carbaldehyde | HCID 86635115 | — |
반응 단계
2H-Indazole-5-carbaldehyde (Stage 150.5, 770 mg, 5.27 mmol) was dissolved in THF (54 mL) and dicyclohexylmethylamine (1.37 mL, 6.32 mmol) was added. After dropwise addition of (2-chloromethoxy-ethyl)-trimethyl-silane (1.21 mL, 6.32 mmol), the RM was stirred for 48 h at rt. It was then taken into EtOAc and washed successively with 0.5 M aqueous NaOH solution and brine. The organic layer was dried on Na2SO4 and evaporated and the residue purified by flash chromatography (CombiFlash® Companion System®, with RediSep® silica gel column, n-hexane/EtOAc=100:0->70:30) to afford white crystals of the title compound (tR 7.14 min (conditions 3), MH+=277).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08822468B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-213deaad1c524c6183a358505892e2ea |
| 출처 메모 | uspto-grants-2014_09 |