Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diazomethane → 5-Bromo-1-diazo-3-(3,4-dichlorophenyl)-2-pentanone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diazomethane | HCID 9550 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | 1-Methyl-2-nitro-1-nitrosoguanidine | HCID 9562060 | — |
| 반응물 | alpha-(2-Bromoethyl)-3,4-dichlorophenylacetic acid chloride | HCID 54519315 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 5-Bromo-1-diazo-3-(3,4-dichlorophenyl)-2-pentanone | HCID 53781276 | — |
반응 단계
Prepare a solution of diazomethane from 15 g of MNNG by reaction with 45 ml of 40% aqueous KOH topped with 150 ml. of Et2O and cool in an ice bath. Add an Et2O solution (40 ml.) of the product of Step 3 (8.2 g, 24.8 mmoles) in small volumes, stir the solution in the ice bath for 15 min, then heat to reflux for 30 min. Remove the solvent in vacuo. Purify the resulting mixture by flash chromatography on silica gel using CH2Cl2 as eluent. Yield: 7.0 g (IR: 2100 cm-1, 1630 cm-1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05696267 |
| 출처 데이터셋 | uspto-grants-1997_12 |
| ORD ID | ord-ae97e286e911405e844d7818b1508d61 |
| 출처 메모 | uspto-grants-1997_12 |