Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Chloromethyl Methyl Ether → Diethyl 1-(methoxymethyl)-2,5-dioxo-4-imidazolylphosphonate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Chloromethyl Methyl Ether | HCID 7864 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Diethyl (2,5-dioxo-2,5-dihydro-1H-imidazol-4-yl)phosphonate | HCID 53733419 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | Diethyl 1-(methoxymethyl)-2,5-dioxo-4-imidazolylphosphonate | HCID 53791991 | — |
반응 단계
To a solution of diethyl 2,5-dioxo-4-imidazolylphosphonate (3.61 g, 0.015 moles) in DMF (10 mL), under N2, is added sodium hydride (80% dispersion in oil) (0.55 g, 0.018 moles) and stirred for 5 minutes. Chloromethyl methyl ether (tech. grade 85%) (1.9 mL, 0.021 moles) is added. This mixture is stirred at room temperature for 4 hours, diluted with ether and ethyl acetate (300 mL) and then washed with water and brine before drying over MgSO4. The aqueous layer is back extracted with methylene chloride and combined with the previous organic fraction. Evaporation of solvents and chromatography (eluant 1% methanol in chloroform) and evaporation under high vacuum affords the required product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05308853 |
| 출처 데이터셋 | uspto-grants-1994_05 |
| ORD ID | ord-b827a0970433490393d7126541b0b1b2 |
| 출처 메모 | uspto-grants-1994_05 |