참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diethyl Oxalate | HCID 7268 | — |
| 반응물 | Ethyl hexanoate | HCID 31265 | — |
| 반응물 | Sodium ethoxide | HCID 2723922 | — |
| 반응물 | Sodium | HCID 5360545 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | Diethyl 2-butyl-3-oxobutanedioate | HCID 251159 | — |
반응 단계
100 ml of ether, then 13.55 ml of diethyl oxalate were added to a solution of sodium ethylate prepared by stirring 2.3 g of sodium and 150 ml of ethanol at 40° C. for one hour. The mixture was refluxed for 15 minutes, cooled down slightly and 50 ml of ethyl caproate were added. The mixture was stirred at ref lux for 3 hours and at 30° C. to 35° C. for 16 hours. 50 ml of water were added and the aqueous phase was separated by decanting, washed twice with ether and acidified with 2N hydrochloric acid. Extraction was carried out 3 times with ether and the combined organic phases were washed with water, then with a saturated solution of sodium chloride, dried and evaporated to dryness to obtain 9.5 g of the desired product which was used as is for the following step.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06004979 |
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| 출처 데이터셋 | uspto-grants-1999_12 |
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| ORD ID | ord-222ce0c246ce4a3e85580fe6cd99ddac |
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| 출처 메모 | uspto-grants-1999_12 |
|---|