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2-Cyanomethyl-6-methoxy-1-tetralone → HCID 12832408、化合物

HRID 1105537
ノート
印刷プレビュー

反応式

HRID 1105537 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 128324072-Cyanomethyl-6-methoxy-1-tetraloneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 12832408HCID 12832408、化合物

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-89e3cfe908904e1f8537e165a33222ba
出典データセット
uspto-grants-1982_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04309345

反応ノート

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