Ethyl Acetate → HCID 21846284, 화합물

HRID 343848노트

반응식

HRID 343848 반응식
[C:1]([C:4]1[CH:12]=[CH:11][CH:10]=[C:9]2[C:5]=1[CH:6]=[CH:7][NH:8]2)(=[O:3])[CH3:2].[H-].[Na+].[C:15](OCC)(=[O:17])[CH3:16]>>[NH:8]1[C:9]2[C:5](=[C:4]([C:1](=[O:3])[CH2:2][C:15](=[O:17])[CH3:16])[CH:12]=[CH:11][CH:10]=2)[CH:6]=[CH:7]1

참가 물질

4

반응물 3

HCID 8857Ethyl AcetateHCID 24758Sodium hydrideHCID 130046731-(1H-Indol-4-yl)ethan-1-one

생성물 1

HCID 21846284HCID 21846284, 화합물

실험 절차

4-Acetylindole (0.101 g) was refluxed in 5 mL of ethyl acetate. Sodium hydride (0.20 g, 60% oil dispersion) was added in portions to the refluxing solution until thin layer chromatography analysis showed complete consumption of the starting material. The reaction mixture was quenched with water and acidified to pH 3. The ethyl acetate layer was dried (magnesium sulfate) and concentrated to give a crude product. The crude material was chromatographed on silica gel, eluting with hexane/ethyl acetate to give 1-(1H-indol-4-yl)-1,3-butanedione (0.104 g), a compound of formula (11), m.p. 104°-105° C.

후처리

  1. customconsumption of the starting material
  2. customThe reaction mixture was quenched with water
  3. dry with materialThe ethyl acetate layer was dried (magnesium sulfate)
  4. concentrationconcentrated
  5. customto give a crude product
  6. customThe crude material was chromatographed on silica gel
  7. washeluting with hexane/ethyl acetate

출처 및 근거

ORD 기록
ord-8801d30994174d00877f81bdb97836c4
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05863924

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