Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → Methyl alpha-Methyl-1-nitro-1,2-dihydro-6-azanaphthalene-2-acetate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | Acetonitrile | HCID 6342 | — |
| 반응물 | 5-Nitroisoquinoline | HCID 69085 | — |
| 반응물 | Tris(dimethylamino)sulfonium difluorotrimethylsilicate | HCID 9795567 | — |
| 용매 | Hexane | HCID 8058 | — |
| 생성물 | Methyl alpha-Methyl-1-nitro-1,2-dihydro-6-azanaphthalene-2-acetate | HCID 13507926 | — |
반응 단계
A flame dried 50 mL flask fitted with an addition funnel was charged with 0.872 g (500 mmol) of 5-nitroisoquinoline and 0.95 mL (5.1 mmol) of MTS. An acetonitrile solution of 1.40 g (5.09 mmol) of TASF was slowly added to the reaction mixture in 15 min at -78° C. The mixture was stirred for 22 h at that temperature. One mL of acetic acid in 5 mL of hexane was added, and reaction was warmed to room temperature. After 30 min, 40 mL of water was added. The solid which precipitated out was collected and analyzed. The product yield was 0.972 g (74%). The product material was analyzed by infrared spectroscopy, nuclear magnetic resonance spectroscopy, and mass spectrometry.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05164499 |
| 출처 데이터셋 | uspto-grants-1992_11 |
| ORD ID | ord-02f61dd96e9b44fa8d5cc71fd42e8da8 |
| 출처 메모 | uspto-grants-1992_11 |