Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → N-Methoxy-N-methyl-4-oxocyclohexanecarboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Oxalyl chloride | HCID 65578 | — |
| 반응물 | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| 반응물 | 4-Oxocyclohexanecarboxylic acid | HCID 192730 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | N-Methoxy-N-methyl-4-oxocyclohexanecarboxamide | HCID 89657356 | 39% |
반응 단계
To a solution of 4-oxocyclohexanecarboxylic acid (4.2 g, 0.0293 mol) in CH2Cl2 (20 mL) was added oxalyl chloride (5.2 g, 0.44 mol) slowly, stirred at room temperature for 1 hour and concentrated, then 20 mL CH2Cl2 was added, followed by addition of Et3N (9 g, 0.116 mol) and N,O-dimethylhydroxylamine hydrochloride (3.5 g, 0.0359 mol). The reaction mixture was stirred for 2 hours, and then 100 mL water was added. The mixture was extracted with ethyl acetate. The extract was concentrated and purified by column chromatography to give the desired product (2.1 g, 39% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09309211B2 |
| 출처 데이터셋 | uspto-grants-2016_04 |
| ORD ID | ord-0c683d434d2342d7a29b14e05751a56a |
| 출처 메모 | uspto-grants-2016_04 |