Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylformamide → 4-Difluoro methoxy-8-nitro-1-formyl dibenzo[b,d]furan
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Sodium Acetate | HCID 517045 | — |
| 반응물 | 4-Difluoromethoxy-3-(4-nitro-2-bromophenoxy)benzaldehyde | HCID 24758282 | — |
| 생성물 | 4-Difluoro methoxy-8-nitro-1-formyl dibenzo[b,d]furan | HCID 21105710 | 73.3% |
반응 단계
To a mixture of 3-(2-bromo-4-nitrophenoxy)-4-(difluoromethoxy)benzaldehyde (11.5 g, 0.030 mol) and sodium acetate (3.7 g, 0.045 mol) in dimethylformamide (50 mL) palladium(II) acetate (0.68 g, 0.003 mol) was added in 4 different lots with 1 hour duration at 120-125° C. After the completion of the addition, it was refluxed for 16 hours. The reaction mixture was filtered through hyflo, washed with dimethylformamide (10 mL). The filtrate was poured into the cold water. The solid separated out was filtered. The solid was washed with hexane and dried. Yield—73.3%. HPLC (purity): 84.5%; Rf—0.5 (Ethyl acetate:Hexane (3:7)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08580795B2 |
| 출처 데이터셋 | uspto-grants-2013_11 |
| ORD ID | ord-e52a30bfcae64afbb41a65f52481ab92 |
| 출처 메모 | uspto-grants-2013_11 |