Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Bicarbonate → 2,4,5-Trimethoxyaniline
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 1,2,4-Trimethoxy-5-nitrobenzene | HCID 822415 | — |
| 반응물 | Tin tetrachloride dihydrate | HCID 85782573 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 2,4,5-Trimethoxyaniline | HCID 12410138 | 54.3% |
반응 단계
1,2,4-Trimethoxy-5-nitro-benzene (1.20 g, 5.63 mmol) and tin chloride dihydrate (3.81 g, 16.9 mmol) in ethyl acetate (50 mL) was stirred at 65-70° C. for 20 h. The reaction was cooled, carefully neutralized with sodium bicarbonate and was filtered through Celite. The organic phase was washed with brine, dried (sodium sulfate) and was evaporated. Purification by flash chromatography (SiO2) eluted with 3:7 ethyl acetate:hexanes provided 2,4,5-trimethoxy-phenylamine (0.56 g, 54% yield) as a tan solid. 1H-NMR (DMSO-d6, 500 MHz) 6.57 (s, 1H), 6.37 (s, 1H), 3.70 (s, 3H), 3.65 (s, 3H), 3.63 (s, 3H) ppm; HPLC (Method A) 2.163 min.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07902239B2 |
| 출처 데이터셋 | uspto-grants-2011_03 |
| ORD ID | ord-a6b536d91ec94f6fbd89326ad637e0d7 |
| 출처 메모 | uspto-grants-2011_03 |