Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanamine, N-methoxy-, hydrochloride (1:1) → 3-tert-Butyl-N-methoxy-N-methyl-5-[3-(tetrahydropyran-2-yloxy)propoxy]benzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | O-[(Ethoxycarbonyl)cyanomethylenamino]-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733286 | — |
| 반응물 | 3-tert-Butyl-5-[3-(tetrahydropyran-2-yloxy)propoxy]benzoic acid | HCID 58136832 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-tert-Butyl-N-methoxy-N-methyl-5-[3-(tetrahydropyran-2-yloxy)propoxy]benzamide | HCID 58136958 | 99.4% |
반응 단계
3-tert-Butyl-5-[3-(tetrahydropyran-2-yloxy)propoxy]benzoic acid (O4.059; 4.90 g) and N,O-dimethylhydroxylaminehydrochloride (1.42 g) were dissolved in DMF (80 ml) and admixed with Hünig's base (4.81 ml) and TOTU (4.78 g). After stirring for 2 h, the mixture was left to stand overnight. Then the DMF was drawn off, the mixture was partitioned between EA and saturated sodium hydrogencarbonate solution, and the EA phase was removed, dried over magnesium sulfate, filtered and concentrated. 5.49 g of the title compound were obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08198272B2 |
| 출처 데이터셋 | uspto-grants-2012_06 |
| ORD ID | ord-aa8b3e8f1c4a4b8c90256da1b6eea2b5 |
| 출처 메모 | uspto-grants-2012_06 |