Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethyl bromoacetate → [1-((S)-2-Benzyloxycarbonylamino-propyl)-7-bromo-1H-indazol-6-yloxy]-acetic acid ethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethyl bromoacetate | HCID 7748 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Benzyl (S)-2-(7-bromo-6-hydroxy-1H-indazol-1-yl)-1-methylethylcarbamate | HCID 136207273 | — |
| 용매 | Acetone | HCID 180 | — |
| 생성물 | [1-((S)-2-Benzyloxycarbonylamino-propyl)-7-bromo-1H-indazol-6-yloxy]-acetic acid ethyl ester | HCID 69253335 | 84.1% |
반응 단계
To a mixture of the compound from Step A (0.90 g, 2.23 mmol), potassium carbonate (0.40 g, 2.90 mmol) in acetone (80 mL) was added ethyl bromoacetate (0.484 g, 0.32 mL, 2.90 mmol) with stirring. The mixture was heated at reflux temperature for 3 h and evaporated to dryness. The residue was mixed with water (100 mL) and extracted with EtOAc (3×60 mL). The combined extracts were dried over magnesium sulfate, filtered and evaporated to dryness. Chromatography on silica eluting with a gradient of 10% to 30% EtOAc/hexane gave a solid (0.92 g, 84%): mp 89-90° C.; LCMS (+APCI) 490, 492 (M+H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07425572B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-25122af1ac5b4d528180be0844a2e284 |
| 출처 메모 | uspto-grants-2008_09 |