Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethyl Acetate → N,N-dimethyl-N-[2-(7-nitro-1H-indazol-4-yl)ethyl]amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Sodium cyanoborohydride | HCID 5003444 | — |
| 반응물 | N,N-dimethyl-N-[2-(7-nitro-1H-indazol-4-yl)ethenyl]amine | HCID 54098844 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | N,N-dimethyl-N-[2-(7-nitro-1H-indazol-4-yl)ethyl]amine | HCID 13629307 | 84.5% |
반응 단계
16.2 g of N,N-dimethyl-N-[2-(7-nitro-1H-indazol-4-yl)ethenyl]amine is dissolved in 200 ml of acetic acid and combined under ice cooling in incremental portions with 6.3 g of sodium cyanoborohydride within 30 minutes. After another 30 minutes, the mixture is combined with ice and ethyl acetate, adjusted to 8-9 with concentrated sodium hydroxide solution, and extracted with ethyl acetate. The solution is dried, concentrated, and the residue recrystallized from ethyl acetate/diisopropyl ether, thus obtaining 13.8 g of N,N-dimethyl-N-[2-(7-nitro-1H-indazol-4-yl)ethyl]amine, mp 145°-146° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04958026 |
| 출처 데이터셋 | uspto-grants-1990_09 |
| ORD ID | ord-42e58cecc7064844bd4c52925edbe81c |
| 출처 메모 | uspto-grants-1990_09 |