Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Benzaldehyde, 3-amino- → 1-(2-Fluoro-5-trifluoromethylphenyl)-3-(3-formylphenyl)urea
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Benzaldehyde, 3-amino- | HCID 74366 | — |
| 반응물 | Potassium bisulfate | HCID 516920 | — |
| 반응물 | 2-Fluoro-5-(trifluoromethyl)phenyl isocyanate | HCID 2733380 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 생성물 | 1-(2-Fluoro-5-trifluoromethylphenyl)-3-(3-formylphenyl)urea | HCID 87362302 | 57% |
반응 단계
A mixture of 484 mg of 3-aminobenzaldehyde (4 mmol) (polymerized form) and 290 μl of 2-fluoro-5-trifluoromethylphenyl isocyanate in 4 ml of DCE is treated in a CEM Discover microwave oven at 100° C. for 10 minutes (power 90). After cooling, the mixture is poured into 100 ml of saturated potassium hydrogen sulfate solution and extracted with twice 50 ml of ethyl acetate. The combined organic phases are washed with water, dried over sodium sulfate and evaporated. 740 mg of the expected aldehyde (yield=57%) are obtained in an LC/MS purity of 82%. The crude product is used directly for the following steps. ([M+H]+): 327. RT=4.28 min (acetonitrile/water gradient from 30% to 90%—Method B).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07989439B2 |
| 출처 데이터셋 | uspto-grants-2011_08 |
| ORD ID | ord-4d5d4efd8a634b739b97bb363588779b |
| 출처 메모 | uspto-grants-2011_08 |