Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethyl malonate → 1,1-Dimethyl 2-ethenylcyclopropane-1,1-dicarboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethyl malonate | HCID 7943 | — |
| 반응물 | 1,4-Dichloro-2-butene, (2E)- | HCID 642197 | — |
| 반응물 | Sodium Methoxide | HCID 10942334 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 1,1-Dimethyl 2-ethenylcyclopropane-1,1-dicarboxylate | HCID 10464992 | 105.8% |
반응 단계
Sodium methoxide (108.02 g, 2.0 moles) 25% in MeOH was added in 40 minutes to dimethyl malonate (132.12 g, 1.0 mole), 1,4-dichlorobutene-2 (150 g, 1.2 moles), and 50 mL MeOH and allowed to stir at ambient temperature overnight. The mixture was vacuum filtered, neutralized with concentrated HCl to 3.5-4.0 pH, and filtered a second time. Solvent was then removed under vacuum to give 194.8 g of light yellow crude product. Vacuum distillation (55°/0.25 mm-72°/0.4 mm) with 0.064 g of hydroquinone added gave 142.5 g of product (77.4% yield) and 30.4 g of residue.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04713478 |
| 출처 데이터셋 | uspto-grants-1987_12 |
| ORD ID | ord-eedc9610040547acb37c82c9c8752e35 |
| 출처 메모 | uspto-grants-1987_12 |