Ethanol → HCID 15533732、化合物

HRID 1280332ノート

反応式

HRID 1280332 の反応式
[Cl-].[C:2]1([NH+:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)N)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:16]1[C:24]2[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=2)[CH2:18][C:17]1=O.C(O)C>O>[C:2]1([N:8]2[C:10]3[C:15](=[CH:14][CH:13]=[CH:12][CH:11]=3)[C:18]3[C:19]4[C:24]([CH2:16][C:17]2=3)=[CH:23][CH:22]=[CH:21][CH:20]=4)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 702EthanolHCID 119832-IndanoneHCID 45073535N,N-Diphenylhydrazinium chloride

生成物 1

HCID 15533732HCID 15533732、化合物収率 45%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

In a 0.25 l bulb were placed 10 g (45 mmol) of N,N-diphenylhydrazinium chloride, 6.0 g (45 mmol) of 2-indanone and 50 ml of ethanol. The thus obtained mixture was heated at reflux for 4 hours and it was poured into water; the residual mixture was extracted with CH2Cl2 (150 ml) and the solvent was evaporated. The wanted compound was isolated by passing the obtained mixture through a column of silicagel, eluting with benzene/hexane=1:2. The resulting solution was evaporated and treated with 10 ml of hexane, obtaining the precipitation of crystals. Said crystals were separated, washed with hexane (10 ml) and finally dried, thus yielding 5.4 g of N-phenyl-5,6-dihydroindeno[2,1-b]indole (yield=45%).

後処理

  1. temperatureThe thus obtained mixture was heated
  2. temperatureat reflux for 4 hours
  3. extractionthe residual mixture was extracted with CH2Cl2 (150 ml)
  4. customthe solvent was evaporated
  5. customThe wanted compound was isolated
  6. washeluting with benzene/hexane=1:2
  7. customThe resulting solution was evaporated
  8. additiontreated with 10 ml of hexane
  9. customobtaining
  10. customthe precipitation of crystals
  11. customwere separated
  12. washwashed with hexane (10 ml)
  13. customfinally dried

出典と根拠

ORDレコード
ord-53ee3f48c1d444c1b94b72dbf47b049b
出典データセット
uspto-grants-2002_09
特許番号
US06451724B1

反応ノート

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