4-Nitrobenzaldehyde → 2,2-Dimethyl-5-[(4-nitrophenyl)methylidene]-1,3-dioxane-4,6-dione

HRID 1256922ノート

反応式

HRID 1256922 の反応式
[N+:1]([C:4]1[CH:11]=[CH:10][C:7]([CH:8]=O)=[CH:6][CH:5]=1)([O-:3])=[O:2].C1(C)C=CC=CC=1.[CH3:19][C:20]1([CH3:28])[O:27][C:25](=[O:26])[CH2:24][C:22](=[O:23])[O:21]1.N1CCCCC1>C(O)(=O)C>[CH3:19][C:20]1([CH3:28])[O:27][C:25](=[O:26])[C:24](=[CH:8][C:7]2[CH:10]=[CH:11][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=2)[C:22](=[O:23])[O:21]1

参加物

6

反応物 4

HCID 5414-NitrobenzaldehydeHCID 1140TolueneHCID 8082PiperidineHCID 162492,2-Dimethyl-1,3-dioxane-4,6-dione

生成物 1

HCID 8242742,2-Dimethyl-5-[(4-nitrophenyl)methylidene]-1,3-dioxane-4,6-dione収率 69.7%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To 4-nitrobenzaldehyde (15.1 g) were added a toluene (180 mL) solution, Meldrum's acid (14.4 g), piperidine (300 μL) and acetic acid (300 μL) at room temperature, and the mixture was stirred for 5 hr. Insoluble material was collected by filtration, and the obtained solid was washed with ethyl acetate (80 mL). The resulting precipitate was collected by filtration to give the title compound (19.3 g) as a pale-yellow solid.

後処理

  1. filtrationInsoluble material was collected by filtration
  2. washthe obtained solid was washed with ethyl acetate (80 mL)
  3. filtrationThe resulting precipitate was collected by filtration

出典と根拠

ORDレコード
ord-73520dfa6d5345e1ba031d845663de3f
出典データセット
uspto-grants-2013_06
特許番号
US08461209B2

反応ノート

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