Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Benzaldehyde, 3-amino- → 1-(2-Fluorophenyl)-3-(3-formylphenyl)urea
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Benzaldehyde, 3-amino- | HCID 74366 | — |
| 반응물 | 2-Fluorophenyl isocyanate | HCID 85588 | — |
| 반응물 | Potassium bisulfate | HCID 516920 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 생성물 | 1-(2-Fluorophenyl)-3-(3-formylphenyl)urea | HCID 87362836 | 83.7% |
반응 단계
The product was prepared as described in Example 2, starting with 484 mg of 3-aminobenzaldehyde (4 mmol) (polymerized form) and 548 mg of 2-fluorophenyl isocyanate in 4 ml of DCE. 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. 864 mg of the expected aldehyde are isolated in the form of a gum, in an LC/MS purity of 77%. A crystallized fraction is obtained after trituration from ethyl ether. 165 mg of solid are isolated ([M+H]+): 259. RT=4.28 min (acetonitrile/water gradient from 5% to 85%—Method B).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07989439B2 |
| 출처 데이터셋 | uspto-grants-2011_08 |
| ORD ID | ord-e6734d39ccd943858850665bcbc48f10 |
| 출처 메모 | uspto-grants-2011_08 |