Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Hydroxybenzotriazole → tert-butyl 2-amino-3-[3-[(E)-2-(4-fluorophenyl)ethenyl]-4-methoxy-1H-indazol-5-yl]-3-oxopropanoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 반응물 | Glycine tert-butyl ester hydrochloride | HCID 2725036 | — |
| 반응물 | 3-[(E)-2-(4-fluorophenyl)-vinyl]-4-methoxy-1H-indazole-5-carboxylic acid | HCID 59797243 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | tert-butyl 2-amino-3-[3-[(E)-2-(4-fluorophenyl)ethenyl]-4-methoxy-1H-indazol-5-yl]-3-oxopropanoate | HCID 68933335 | — |
반응 단계
3-[(E)-2-(4-Fluorophenyl)-vinyl]-4-methoxy-1H-indazole-5-carboxylic acid obtained by Example 234 and 258 mg of glycine ter-butyl ester hydrochloride were dissolved in 20 mL of N,N-dimethylformamide, and 0.871 mL of diisopropylethylamine and 235 mg of 1-hydroxybenzotriazole were added, and stirred at room temperature for 10 minutes. After cooling to 0° C., 491 mg of WSC hydrochloride was added, and stirred overnight at room temperature. After adding ice water to stop the reaction, the solution was extracted with ethyl acetate. The organic phase was washed with water and saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated, to afford 547 mg of the title compound as pale green crystals.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07429609B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-6799921308ed475b8a1e13d23b8d1121 |
| 출처 메모 | uspto-grants-2008_09 |