Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 3-[(Bicyclo[2.2.1]hept-5-en-2-yl)(hydroxy)methyl]oxolan-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Bicyclo(2.2.1)hept-5-ene-2-carboxaldehyde | HCID 95117 | — |
| 반응물 | 2(3H)-Furanone, 3-bromodihydro- | HCID 95463 | — |
| 촉매 | Zinc | HCID 23994 | — |
| 용매 | Hexane | HCID 8058 | — |
| 생성물 | 3-[(Bicyclo[2.2.1]hept-5-en-2-yl)(hydroxy)methyl]oxolan-2-one | HCID 18345689 | 71.2% |
반응 단계
Addition reaction was carried out by mixing 98 g of zinc powder, 247 g of α-bromo-γ-butyrolactone, 122 g of 5-norbornene-2-carbaldehyde, and 2 kg of dry tetrahydrofuran and heating the mixture under reflux for 10 hours in a nitrogen atmosphere. The reaction mixture was cooled, to which dilute hydrochloric acid was added for neutralization and hexane was added for extraction. The organic layer was washed with water, dried over anhydrous sodium sulfate, filtered, and concentrated in vacuum. Purification by silica gel column chromatography yielded 148 g (yield 71%) of α-[hydroxy(5-norbornen-2-yl)methyl]-γ-butyrolactone.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06500961B2 |
| 출처 데이터셋 | uspto-grants-2002_12 |
| ORD ID | ord-7d6786bc9e194b04a280c19ded1b9c6b |
| 출처 메모 | uspto-grants-2002_12 |