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4-Chlorobenzaldehyde → HCID 178458262、化合物

HRID 1418056
ノート
印刷プレビュー

反応式

HRID 1418056 の反応式
[CH2:1]([O:4][C:5]1[CH:10]=[C:9]([O:11][CH2:12][CH2:13][CH3:14])[CH:8]=[CH:7][C:6]=1[C:15](=O)[C:16]([C:18]1[CH:23]=[CH:22][N:21]=[CH:20][CH:19]=1)=O)[CH2:2][CH3:3].C([O-])(=O)C.[NH4+:29].[Cl:30][C:31]1[CH:38]=[CH:37][C:34]([CH:35]=O)=[CH:33][CH:32]=1.[OH-].[NH4+:40]>C(O)(=O)C.C(OCC)(=O)C>[Cl:30][C:31]1[CH:38]=[CH:37][C:34]([C:35]2[NH:29][C:16]([C:18]3[CH:23]=[CH:22][N:21]=[CH:20][CH:19]=3)=[C:15]([C:6]3[CH:7]=[CH:8][C:9]([O:11][CH2:12][CH2:13][CH3:14])=[CH:10][C:5]=3[O:4][CH2:1][CH2:2][CH3:3])[N:40]=2)=[CH:33][CH:32]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 77264-ChlorobenzaldehydeHCID 14923Ammonium HydroxideHCID 517165Ammonium AcetateHCID 53632863HCID 53632863、化合物

生成物 1

HCID 178458262HCID 178458262、化合物収率 30%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒
HCID 8857
Ethyl Acetate
溶媒

反応条件

温度
0 °C

実験手順

A solution of 1-(2,4-di-n-propyloxyphenyl)-2-(4-pyridyl)ethane-1,2-dione from Step D (61 mg, 0.19 mmol), ammonium acetate (144 mg, 1.87 mmol) and 4-chlorobenzaldehyde (33 mg, 0.23 mmol) in acetic acid (1.5 mL) was heated to 100° C. for 3.5 h. After cooling to 0° C., the ice (4g), ethyl acetate (2 mL) and a concentrated solution of ammonium hydroxide was added until the pH was 10. The layers were separated and the aqueous layer extracted with ethyl acetate. The combined organic extracts were successively washed with water and saturated salt solution and dried over anhydrous sodium sulfate. The mixture was filtered and the solvent removed by rotoevaporation. The residue was purified by flash column chromatography on silica gel eluted with 0-3% methanol in methylene chloride to yield the title compound as a cream-colored solid (25 mg, 30% yield), mass spectrum (CI) m/e=448 (M+1)+.

後処理

  1. customThe layers were separated
  2. extractionthe aqueous layer extracted with ethyl acetate
  3. washThe combined organic extracts were successively washed with water and saturated salt solution
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationThe mixture was filtered
  6. customthe solvent removed by rotoevaporation
  7. customThe residue was purified by flash column chromatography on silica gel
  8. washeluted with 0-3% methanol in methylene chloride

出典と根拠

ORDレコード
ord-dea4770b36114084b3806b9f609720f1
出典データセット
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05880139

反応ノート

読み込み中…

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