Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → (4-Aminophenyl)dimethylphosphine oxide hydrochloride
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | 1-(Dimethyl-phosphinoyl)-4-nitro-benzene | HCID 21897912 | — |
| 촉매 | Palladium | HCID 23938 | — |
| 생성물 | (4-Aminophenyl)dimethylphosphine oxide hydrochloride | HCID 21897911 | — |
반응 단계
A suspension of 1-(Dimethyl-phosphinoyl)-4-nitro-benzene (2.04 g, 10.2 mmol) and 10% palladium on carbon (0.411 g) in 103 mL of absolute EtOH containing 1.15 mL (11.4 mmol) of conc. HCl was flushed with H2 and stirred at ambient temperature (H2 balloon) for 2 h. The reaction mixture was filtered through Celite, the Celite washed with EtOH, and the combined filtrates concentrated to provide the crude product. Recrystallization from boiling iPrOH (10 mL) provided, after several crops, 1.17 g of an off-white solid: 1H NMR (300 MHz, DMSO-d6) δ 7.61 (dd, J-=11.1, 8.4 Hz, 2H), 7.04 (dd, J=8.4, 2.0 Hz, 2H), 1.64 (s, 3H), 1.60 (s, 3H). 31P NMR (121 MHz, DMSO-d6) δ 39.299.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06706699B2 |
| 출처 데이터셋 | uspto-grants-2004_03 |
| ORD ID | ord-77a666d286ac4a32a05e63399ff51bdf |
| 출처 메모 | uspto-grants-2004_03 |