Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → Ethyl 3-(3-chloro-2-fluorophenyl)-2-diazo-3-oxopropanoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 4-Acetamidobenzenesulfonyl azide | HCID 5129185 | — |
| 반응물 | Ethyl 3-(3-chloro-2-fluorophenyl)-3-oxopropanoate | HCID 64717392 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | Ethyl 3-(3-chloro-2-fluorophenyl)-2-diazo-3-oxopropanoate | HCID 86659989 | — |
반응 단계
Ethyl 3-(3-chloro-2-fluorophenyl)-3-oxopropanoate (1.30 g, 5.31 mmol), triethylamine (0.618 g, 6.11 mmol, 1.15 equiv), and 4-acetamidobenzenesulfonyl azide (1.40 g, 5.85 mmol, 1.1 equiv) were combined in acetonitrile (15 mL). After stirred at ambient temperature for 30 minutes, the mixture was concentrated in vacuo and the residue was treated with sodium hydroxide (25 mL, 2 M aqueous) and extracted with twice chloroform. The combined organic extracts were washed once with brine, dried with sodium sulfate, filtered and concentrated in vacuo. The residue was purified by silica gel gradient chromatography (100:0 to 40:60; hexanes:ethyl acetate), providing the titled compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08653079B2 |
| 출처 데이터셋 | uspto-grants-2014_02 |
| ORD ID | ord-85b62a5695854a139211369c4df8ff2b |
| 출처 메모 | uspto-grants-2014_02 |