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 1 N 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 | US04254282 |
| 출처 데이터셋 | uspto-grants-1981_03 |
| ORD ID | ord-9d624b05b78948a99ddc37caee548017 |
| 출처 메모 | uspto-grants-1981_03 |