Hydrochloric Acid → 5,6,7,8-Tetrahydro-2-naphthylamine

HRID 260679

反応式

HRID 260679 の反応式
[N+:1]([C:4]1[CH:13]=[C:12]2[C:7]([CH2:8][CH2:9][CH2:10][C:11]2=O)=[CH:6][CH:5]=1)([O-])=O.O.Cl.[H][H]>C(O)C.[Pd]>[NH2:1][C:4]1[CH:5]=[CH:6][C:7]2[CH2:8][CH2:9][CH2:10][CH2:11][C:12]=2[CH:13]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 384457-Nitro-1-tetraloneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 751935,6,7,8-Tetrahydro-2-naphthylamine収率 86,687.797%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

7-Nitrotetralone (20.0 9, 0.105 mmol) was dissolved in 400 ml of ethanol, and 40 ml of water, 10 ml of concentrated HCl, and 4.0 g of 10% palladium on carbon were added. The reaction mixture was reacted with hydrogen at 30-40 psi for 16 hours. Following hydrogenation, the reaction mixture was filtered and the solvents were evaporated, yielding white crystals. The crystals were washed with acetone, dissolved in cold 10% NaOH, and extracted with EtOAc (3 x). The combined organic layers were washed with water, dried over Na2SO4, filtered and evaporated, to give 2-amino-5,6,7,8-tetrahydronaphthalene (13.4 g, 87.1% yield) as a brown oil.

後処理

  1. filtrationthe reaction mixture was filtered
  2. customthe solvents were evaporated
  3. customyielding white crystals
  4. washThe crystals were washed with acetone
  5. dissolutiondissolved in cold 10% NaOH
  6. extractionextracted with EtOAc (3 x)
  7. washThe combined organic layers were washed with water
  8. dry with materialdried over Na2SO4
  9. filtrationfiltered
  10. customevaporated

出典と根拠

ORDレコード
ord-280fa59257694b5ea051f2cc2b3a6855
出典データセット
uspto-grants-1996_06
特許番号
US05530005

関連ノート

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