Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Stannous chloride dihydrate → 3,5-Dichloro-4-methylaniline
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Stannous chloride dihydrate | HCID 61436 | — |
| 반응물 | 1,3-Dichloro-2-methyl-5-nitrobenzene | HCID 251670 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 3,5-Dichloro-4-methylaniline | HCID 641154 | 80% |
반응 단계
Dissolve 1,3-dichloro-2-methyl-5-nitrobenzene (0.50 g, 2.43 mmol) in DMF and treat with tin (II) chloride dihydrate (2.74 g, 12.1 mmol) in a single portion. Stir the reaction for 1 hour, dilute with ethyl acetate, and filter through celite. Wash the filtrate four times with water and twice with brine, dry over MgSO4, filter and concentrate to a dark oil. Purify the residue by silica gel chromatography eluting with a gradient of 5% to 10% ethyl acetate in hexanes to give 342 mg (80%) of the titled product as white flakes.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07994176B2 |
| 출처 데이터셋 | uspto-grants-2011_08 |
| ORD ID | ord-92bd0f78ff0d4fe28be43870e0a3aee5 |
| 출처 메모 | uspto-grants-2011_08 |