Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetonitrile → HCID 57447078, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetonitrile | HCID 6342 | — |
| 반응물 | Sodium Azide | HCID 33557 | — |
| 반응물 | Cerium trichloride heptahydrate | HCID 21585214 | — |
| 반응물 | Ethyl 4-[(2-chloro-5,6-dimethyl-3-nitropyridin-4-yl)amino]butyrate | HCID 57455392 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 57447078 | HCID 57447078 | 72.3% |
반응 단계
Ethyl 4-[(2-chloro-5,6-dimethyl-3-nitropyridin-4-yl)amino]butyrate (86.2 g, 0.276 mol), sodium azide (35.49 g, 0.552 mol), and cerium chloride heptahydrate (50.86 g, 0.138 mol) were triturated in a 9:1 mixture of acetonitrile:water (1012 mL). The reaction mixture was stirred and heated to reflux for 18 hours. The reaction was filtered and the yellow filtrate was concentrated under reduced pressure to yield 90.94 g of crude product. The material was triturated at 95° C. with 360 mL ethyl acetate and filtered. The filtrate produced pale yellow crystals at ambient temperature to afford 64.3 g of ethyl 4-[(5,6-dimethyl-8-nitrotetrazolo[1,5-a]pyridin-7-yl)amino]butyrate as a yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09328110B2 |
| 출처 데이터셋 | uspto-grants-2016_05 |
| ORD ID | ord-a69fc5e1657b48da89de1763916b591b |
| 출처 메모 | uspto-grants-2016_05 |