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Ethyl benzoylacetate → HCID 22664979, 화합물

HRID 392588
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HRID 392588 반응식
I[CH:2]([CH3:6])[CH:3](I)[CH3:4].C(=O)([O-])[O-].[Na+].[Na+].[CH2:13]([O:15][C:16](=[O:26])[CH2:17][C:18](=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH3:14]>CN(C)C=O>[C:18]([C:17]1([C:16]([O:15][CH2:13][CH3:14])=[O:26])[CH2:4][CH2:3][CH2:2][CH2:6]1)(=[O:25])[C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7170Ethyl benzoylacetateHCID 10340Sodium CarbonateHCID 230423272,3-Diiodobutane

생성물 1

HCID 22664979HCID 22664979, 화합물수율 58.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
57.5 °C

실험 절차

Diiodobutane (17.1 g, 55 mmol), sodium carbonate (35 g, 330 mmol), ethylbenzoylacetate (10.6 g, 55 mmol) and dimethylformamide (170 ml) were mixed and the mixture was stirred at 55 to 60° C. overnight. The mixture after completion of reaction was poured into ice water and the mixture was extracted twice with ethyl acetate (100 ml). The extract was dried over sodium sulfate, and after concentration, purified by silica gel column chromatography (hexane:ethyl acetate=9:1) to give the title compound (7.9 g, 58%) as a colorless oil.

후처리

  1. customThe mixture after completion of reaction
  2. extractionthe mixture was extracted twice with ethyl acetate (100 ml)
  3. dry with materialThe extract was dried over sodium sulfate
  4. concentrationafter concentration
  5. custompurified by silica gel column chromatography (hexane:ethyl acetate=9:1)

출처 및 근거

ORD 기록
ord-df9244668d0f45f2a8310bb2a704043d
출처 데이터셋
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06800778B1

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