Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Stannous chloride dihydrate → Methyl 3-amino-6-chloro-2-methylbenzoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Stannous chloride dihydrate | HCID 61436 | — |
| 반응물 | HCID 68749648 | HCID 68749648 | — |
| 반응물 | Methyl 6-chloro-2-methyl-3-nitrobenzoate | HCID 68754758 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | Methyl 3-amino-6-chloro-2-methylbenzoate | HCID 21710154 | — |
반응 단계
To above stirred mixture of methyl 6-chloro-2-methyl-3-nitrobenzoate 62 and methyl 6-chloro-2-methyl-5-nitrobenzoate in EtOH (500 mL), SnCl2.2H2O (224 g, 992 mmol, 4 eq) was added and the resulting mixture was stirred at reflux for 3 h. The reaction mixture was allowed to cool to RT and concentrated in vacuo. The residue was poured into water (1 L) and extracted with ethyl acetate (5×500 mL). The combined organic layers were washed with brine, dried over Na2SO4 and filtered. The filtrate was concentrated in vacuo and the residue was purified by flash column chromatography on silica gel (2-10% ethyl acetate-hexanes) to afford the regio-isomer methyl 3-amino-6-chloro-2-methylbenzoate 63.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08901133B2 |
| 출처 데이터셋 | uspto-grants-2014_12 |
| ORD ID | ord-122799ea107049a5906d6fad7e1c3743 |
| 출처 메모 | uspto-grants-2014_12 |