Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylformamide → 3-[(Tert-butoxy)carbonyl]-5-nitrobenzoic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | 5-Nitroisophthalic acid | HCID 12069 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 3-[(Tert-butoxy)carbonyl]-5-nitrobenzoic acid | HCID 69381087 | 248.8% |
반응 단계
To a suspension of 5-nitro-isophthalic acid (5.0 g, 23.7 mmol) in dry toluene (100 ml) at 110° C. was added dimethylformamide di-t-butylacetale (3.4 ml, 71 mmol) drop wise over 60 min. Heating was continued for 45 min and the reaction mixture was left at Rt over night. The precipitated starting material was removed by filtration. The filtrate was concentrated to give a yellow oil (7.88 g). This was purified by flash chromatography using EtOAc/Hept 1:2 and EtOAc/Hept 1:2+5% AcOH in two portions to give the title compound in 38% yield (2.38 g)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08067362B2 |
| 출처 데이터셋 | uspto-grants-2011_11 |
| ORD ID | ord-43d77f5ddfbd4af4bf35a78f513804a3 |
| 출처 메모 | uspto-grants-2011_11 |