Acetic Acid → 2-(4-Hydroxy-3-nitrobenzylidene)acetylacetone

HRID 255705

반응식

HRID 255705 반응식
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=O)=[CH:4][C:3]=1[N+:10]([O-:12])=[O:11].[C:13]([CH2:16][C:17](=[O:19])[CH3:18])(=[O:15])[CH3:14].C(O)(=O)C.N1CCCCC1>C1C=CC=CC=1.C(OCC)C>[OH:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[CH:14][C:13]([CH2:16][C:17](=[O:19])[CH3:18])=[O:15])=[CH:4][C:3]=1[N+:10]([O-:12])=[O:11]

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 8082PiperidineHCID 181694-Hydroxy-3-nitrobenzaldehydeHCID 31261Acetylacetone

생성물 1

HCID 570301622-(4-Hydroxy-3-nitrobenzylidene)acetylacetone수율 85%

시약·촉매·용매 2

HCID 241Benzene용매HCID 3283Diethyl Ether용매

실험 절차

A mixture of 4-hydroxy-3-nitrobenzaldehyde (43.5 g), acetylacetone (26 g), acetic acid (3.12 g) and piperidine (1.03 ml) in benzene (26 ml) was refluxed for 1 hours under azeotropic dehydration. To the reaction mixture was added 100 ml of diethyl ether. The mixture was washed with water (100 ml) and a saturated aqueous solution of sodium chloride (50 ml), dried over magnesium sulfate and evaporated in vacuo to afford 2-(4-hydroxy-3-nitrobenzylidene)acetylacetone (55.0 g).

후처리

  1. temperaturewas refluxed for 1 hours under azeotropic dehydration
  2. washThe mixture was washed with water (100 ml)
  3. dry with materiala saturated aqueous solution of sodium chloride (50 ml), dried over magnesium sulfate
  4. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-5b3fcac77b6a4e28a7a55070daa8b947
출처 데이터셋
uspto-grants-1987_10
특허 번호
US04698340

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