Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
3-Methyl-2-buten-1-OL → 3-Methylbut-2-en-1-yl 3-oxobutanoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 3-Methyl-2-buten-1-OL | HCID 11173 | — |
| 반응물 | Diketene | HCID 12661 | — |
| 촉매 | Sodium Acetate | HCID 517045 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 3-Methylbut-2-en-1-yl 3-oxobutanoate | HCID 4173429 | 76% |
반응 단계
A mixture of 3-methyl-2-buten-1-ol (21.2 g, 0.25 mole) and anhydrous sodium acetate (0.1 g) was cooled to 0°. Diketene (36 ml, 0.3 mole) was added dropwise over a period of 1.5 to 2 hours. The reaction mixture was then heated to 75°-80°, and this temperature was maintained for one hour. The mixture was diluted with ether. The ethereal solution was washed successively with aqueous 1N hydrochloric acid, saturated aqueous sodium bicarbonate, saturated aqueous sodium chloride, and then dried over magnesium sulfate. The ether was evaporated, leaving a residue which was distilled under vacuum, affording 3-methyl-2-butenyl acetoacetate (32.1 g, 76% yield); bp 114°-117°/18-19 mm.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04526987 |
| 출처 데이터셋 | uspto-grants-1985_07 |
| ORD ID | ord-37d5d49cff774245a8baa9ec84d61fbb |
| 출처 메모 | uspto-grants-1985_07 |