Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-(Allyloxy)-2-methyl-1-oxopropan-2-yl 2-chloro-5-nitrobenzoate → 5-Amino-2-chlorobenzoic acid 1-allyloxycarbonyl-1-methyl-ethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-(Allyloxy)-2-methyl-1-oxopropan-2-yl 2-chloro-5-nitrobenzoate | HCID 11782392 | — |
| 반응물 | HCID 178418361 | HCID 178418361 | — |
| 촉매 | Tetramethylammonium chloride | HCID 6379 | — |
| 용매 | Methyl Ethyl Ketone | HCID 6569 | — |
| 생성물 | 5-Amino-2-chlorobenzoic acid 1-allyloxycarbonyl-1-methyl-ethyl ester | HCID 10968509 | 96.8% |
반응 단계
In a stirred autoclave, 0.33 g of a catalyst prepared according to Example H1 is added to a solution of 65.5 g of allyl 2-(2-chloro-5-nitrobenzoyloxy)-2-methylpropionate in 370 g of methyl ethyl ketone, 0.2 g (0.5 mol %) of FeCl2 4H2O and 22 mg (0.1 mol %) of tetramethylammonium chloride are added in addition, and the mixture is hydrogenated for 5 hours at a temperature of 140° C. and at a hydrogen pressure of 15 bar. After cooling and flushing the stirred autoclave with nitrogen, the catalyst is filtered off and rinsed with 40 g of methyl ethyl ketone. 435.5 g are obtained of a solution having a content of 13.22% of allyl 2-(2-chloro-5-aminobenzoyloxy)-2-methylpropionate (yield: 96.8 % of theory).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05856578 |
| 출처 데이터셋 | uspto-grants-1999_01 |
| ORD ID | ord-06bc6bfbc348432182bf7365f30b09d3 |
| 출처 메모 | uspto-grants-1999_01 |