Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → N,N'-dimethoxy-N,N'-dimethylbutanediamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Succinyl chloride | HCID 10970 | — |
| 반응물 | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| 생성물 | N,N'-dimethoxy-N,N'-dimethylbutanediamide | HCID 4379853 | — |
반응 단계
Dissolve 136.2 g of succinyl dichloride and 180.0 g N,O-dimethylhydroxylamine hydrochloride in 1.2 L dichloromethane and cool it in an ice bath. Add 305.9 g pyridine from an addition funnel with stir over 1.5 hours. Let the reaction mixture warm up to room temperature over night. Pour the reaction mixture into ice and water and separate the layers. Wash the organic layer with cold 2 N HCl (2×), water, 5% NaHCO3 (2×), and saturated brine. Dry over anhydrous Na2SO4 and evaporate to give crude product. It was washed with 3:1 hexanes and dichloromethane and dried to give the title compound as a light tan solid 1H NMR (CDCl3, 500 MHz δ: 3.70 (s, 6H), 3.15 (s, 6H), 2.74 (s, 4H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07528163B2 |
| 출처 데이터셋 | uspto-grants-2009_05 |
| ORD ID | ord-7fe6b6bc418f4397a56f52d339a64eeb |
| 출처 메모 | uspto-grants-2009_05 |