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2-Cyanomethyl-6-methoxy-1-tetralone → HCID 12832408, 화합물

HRID 46511
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인쇄 미리보기

반응식

HRID 46511 반응식
[C:1]([CH2:3][CH:4]1[CH2:13][CH2:12][C:11]2[C:6](=[CH:7][CH:8]=[C:9]([O:14][CH3:15])[CH:10]=2)[C:5]1=O)#[N:2].[H][H]>C(O)C.[Ni]>[CH3:15][O:14][C:9]1[CH:8]=[CH:7][C:6]2[C:5]3[CH:4]([CH2:3][CH2:1][N:2]=3)[CH2:13][CH2:12][C:11]=2[CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 128324072-Cyanomethyl-6-methoxy-1-tetraloneHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 12832408HCID 12832408, 화합물

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

The solution of 50 g of 2-cyanomethyl-6-methoxy-1-tetralone in 1000 ml of ethanol is hydrogenated in the presence of 15 g of Raney nickel at atmospheric pressure and room temperature until 2 mole equivalents of hydrogen are consumed. The mixture is filtered, the filtrate evaporated and the crude product dissolved in 500 ml of N hydrochloric acid. The solution is washed with diethyl ether, treated with charcoal, filtered and the filtrate is basified with 3 N aqueous sodium hydroxide. It is extracted with methylene chloride, the extract dried, evaporated, the residue crystallized from petroleum ether and recrystallized from hexane, to yield the 7-methoxy-3,3a,4,5-tetrahydro-2H-benz[g]indole melting at 102°-104°.

후처리

  1. customare consumed
  2. filtrationThe mixture is filtered
  3. customthe filtrate evaporated
  4. dissolutionthe crude product dissolved in 500 ml of N hydrochloric acid
  5. washThe solution is washed with diethyl ether
  6. additiontreated with charcoal
  7. filtrationfiltered
  8. extractionIt is extracted with methylene chloride
  9. customthe extract dried
  10. customevaporated
  11. customthe residue crystallized from petroleum ether
  12. customrecrystallized from hexane

출처 및 근거

ORD 기록
ord-0807c7593680411f946d5c35a4e930f9
출처 데이터셋
uspto-grants-1979_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04173633

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