Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,3-Dioxolane-4-methanol → 1,3-Dioxan-5-yl 5-norbornene-2-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,3-Dioxolane-4-methanol | HCID 21618 | — |
| 반응물 | Methyl bicyclo[2.2.1]hept-5-ene-2-carboxylate | HCID 250075 | — |
| 반응물 | Sodium Methoxide | HCID 10942334 | — |
| 반응물 | (1,3-Dioxolan-4-yl)methyl 5-norbornene-2-carboxylate | HCID 22713062 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 1,3-Dioxan-5-yl 5-norbornene-2-carboxylate | HCID 69910200 | 93% |
반응 단계
A mixture of 104 g of glycerol formal, 152 g of methyl 5-norbornene-2-carboxylate, 2.0 g of sodium methoxide and 300 ml of toluene was heated under reflux for 5 hours while gradually distilling off methanol formed during the reaction. After cooling, the reaction solution was washed with saturated sodium bicarbonate water, dried over anhydrous sodium sulfate, and concentrated in vacuum. It was further purified by vacuum distillation, obtaining 209 g of a mixture of (1,3-dioxolan-4-yl)methyl 5-norbornene-2-carboxylate and 1,3-dioxan-5-yl 5-norbornene-2-carboxylate (boiling point 111-115° C./530 Pa, yield 93%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06743566B2 |
| 출처 데이터셋 | uspto-grants-2004_06 |
| ORD ID | ord-fff2a3c571664cd69e5568bf0402cb1f |
| 출처 메모 | uspto-grants-2004_06 |