1,3-Indandione → 2-(3,4-dichlorobenzylidene)-1H-indene-1,3(2H)-dione

HRID 490786

反応式

HRID 490786 の反応式
[C:1]1(=[O:11])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3](=[O:10])[CH2:2]1.[Cl:12][C:13]1[CH:14]=[C:15]([CH:18]=[CH:19][C:20]=1[Cl:21])[CH:16]=O>CCO.N1CCCCC1>[Cl:12][C:13]1[CH:14]=[C:15]([CH:18]=[CH:19][C:20]=1[Cl:21])[CH:16]=[C:2]1[C:1](=[O:11])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]1=[O:10]

参加物

5

反応物 2

HCID 118151,3-IndandioneHCID 227103,4-Dichlorobenzaldehyde

生成物 1

HCID 75149132-(3,4-dichlorobenzylidene)-1H-indene-1,3(2H)-dione収率 85%

試薬・触媒・溶媒 2

HCID 8082Piperidine触媒HCID 702Ethanol溶媒2 回

実験手順

To a solution of indan-1,3-dione (1a) (960 mg, 6.6 mmol) in EtOH (8.2 mL) was added 3,4-dichlorobenzaldehyde (b) (1.3 g 7.2 mmol) followed by piperidine (3 drops). The reaction mixture was heated to reflux for 30 min. After cooling the reaction was diluted with EtOH (8 mL) and the precipitate was filtered. The resulting solid was triturated twice with EtOH and dried under high vacuum to give 2-(3,4-dichloro-benzylidene)-indane-1,3-dione (1c) (1.7 g, 82% yield).

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 30 min
  3. temperatureAfter cooling the reaction
  4. filtrationthe precipitate was filtered
  5. customThe resulting solid was triturated twice with EtOH
  6. customdried under high vacuum

出典と根拠

ORDレコード
ord-3fe82cce85a548b6a1decef4096f02d3
出典データセット
uspto-grants-2009_05
特許番号
US07528167B2

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