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

HRID 255705

反応式

HRID 255705 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

HCID 570301622-(4-Hydroxy-3-nitrobenzylidene)acetylacetone収率 85%

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 3283Diethyl Ether溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-5b3fcac77b6a4e28a7a55070daa8b947
出典データセット
uspto-grants-1987_10
特許番号
US04698340

関連ノート

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