Ethanol → HCID 15533732, 화합물

HRID 1280332노트

반응식

HRID 1280332 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 15533732HCID 15533732, 화합물수율 45%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-53ee3f48c1d444c1b94b72dbf47b049b
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06451724B1

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