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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Diethyl Oxalate → Diethyl 2-butyl-3-oxobutanedioate

HRID 612435
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HRID 612435 반응식
[C:1]([O:8][CH2:9][CH3:10])(=[O:7])[C:2]([O:4]CC)=O.CC[O-].[Na+].[Na].[C:16]([O:23][CH2:24][CH3:25])(=[O:22])[CH2:17][CH2:18][CH2:19][CH2:20][CH3:21]>O.C(O)C.CCOCC>[CH2:18]([CH:17]([C:2](=[O:4])[C:1]([O:8][CH2:9][CH3:10])=[O:7])[C:16]([O:23][CH2:24][CH3:25])=[O:22])[CH2:19][CH2:20][CH3:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 7268Diethyl OxalateHCID 31265Ethyl hexanoateHCID 2723922Sodium ethoxideHCID 5360545Sodium

생성물 1

HCID 251159Diethyl 2-butyl-3-oxobutanedioate

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962
Water
용매
HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

  1. customprepared
  2. temperatureThe mixture was refluxed for 15 minutes
  3. temperaturecooled down slightly
  4. customthe aqueous phase was separated
  5. customby decanting
  6. washwashed twice with ether
  7. extractionExtraction
  8. washthe combined organic phases were washed with water
  9. dry with materialwith a saturated solution of sodium chloride, dried
  10. customevaporated to dryness

출처 및 근거

ORD 기록
ord-222ce0c246ce4a3e85580fe6cd99ddac
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06004979

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