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Ethyl Acetoacetate → HCID 10176552, 화합물

HRID 1699990
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HRID 1699990 반응식
[C:1]([O:7][CH2:8][CH3:9])(=[O:6])[CH2:2][C:3]([CH3:5])=[O:4].[H-].[Na+].Cl[CH2:13][CH:14]=[C:15]([CH3:17])[CH3:16]>CN(C)C=O>[CH2:8]([O:7][C:1](=[O:6])[CH:2]([C:3](=[O:4])[CH3:5])[CH2:13][CH:14]=[C:15]([CH3:17])[CH3:16])[CH3:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8868Ethyl AcetoacetateHCID 104291-Chloro-3-methyl-2-buteneHCID 24758Sodium hydride

생성물 1

HCID 10176552HCID 10176552, 화합물수율 58.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

To a solution of 26.05 g ethyl acetoacetate in 150 ml of dimethylformamide, 8.30 g 60% sodium hydride were added portionwise over 1 hour while the temperature rose to 60° C. After cooling down to room temperature, a solution of 24.8 g 1-chloro-3-methyl-2-butene in 50 ml of dimethylformamide was dropped in. Then the mixture was stirred at room temperature for 2.5 hours. The mixture was quenched with water and extracted with ether. The combined organic phase was dried, filtered and evaporated to dryness. The resulting yellow oil was purified by distillation to yield 23.16 g of a colourless oil.

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후처리

  1. customrose to 60° C
  2. customThe mixture was quenched with water
  3. extractionextracted with ether
  4. customThe combined organic phase was dried
  5. filtrationfiltered
  6. customevaporated to dryness
  7. distillationThe resulting yellow oil was purified by distillation

출처 및 근거

ORD 기록
ord-ad03808fc6114408a3014ea70dc3e323
출처 데이터셋
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06348618B1

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