Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Malononitrile → Methyl 3-(dicyanomethyl)tetrahydrofuran-3-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Malononitrile | HCID 8010 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Methyl 3-bromotetrahydrofuran-3-carboxylate | HCID 66653660 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Methyl 3-(dicyanomethyl)tetrahydrofuran-3-carboxylate | HCID 86689276 | — |
반응 단계
440 mg (11.00 mmol) of sodium hydride (60% in mineral oil) were initially charged in 30 ml of THF, and 726 mg (11.00 mmol) of malononitrile were added in portions. Thereafter, 2.3 g (11.00 mmol) of the compound obtained in example 11A in THF (50 ml) were added. The mixture was stirred at RT for 6 h and then heated to 50° C. overnight. After cooling, the mixture was admixed with saturated aqueous sodium hydrogencarbonate solution and extracted three times with ethyl acetate. The combined organic phases were washed with saturated aqueous sodium chloride solution and then dried over sodium sulfate, filtered and concentrated. The residue (2.66 g) was dried under high vacuum for 1 h and then converted without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08765769B2 |
| 출처 데이터셋 | uspto-grants-2014_07 |
| ORD ID | ord-9e968955856e4e3fabd83b50d7d5a609 |
| 출처 메모 | uspto-grants-2014_07 |