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2-Methoxyphenethylamine → 5,6,7,8-Tetrahydro-5-[[2-(2-methoxyphenyl)ethyl]amino]-2-quinolinecarbonitrile

HRID 875304
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HRID 875304 반응식
O=[C:2]1[CH2:11][CH2:10][CH2:9][C:8]2[N:7]=[C:6]([C:12]#[N:13])[CH:5]=[CH:4][C:3]1=2.[CH3:14][O:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[CH2:22][CH2:23][NH2:24].O.C1(C)C=CC(S(O)(=O)=O)=CC=1.[BH4-].[Na+]>C1(C)C=CC=CC=1.O>[CH3:14][O:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[CH2:22][CH2:23][NH:24][CH:2]1[CH2:11][CH2:10][CH2:9][C:8]2[N:7]=[C:6]([C:12]#[N:13])[CH:5]=[CH:4][C:3]1=2
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참가 물질

7

반응물 4

HCID 748962-MethoxyphenethylamineHCID 521998p-Toluenesulfonic acid monohydrateHCID 4311764Sodium borohydrideHCID 867098005-Oxo-5,6,7,8-tetrahydroquinoline-2-carbonitrile

생성물 1

HCID 899408535,6,7,8-Tetrahydro-5-[[2-(2-methoxyphenyl)ethyl]amino]-2-quinolinecarbonitrile

시약·촉매·용매 2

HCID 962
Water
용매
HCID 1140Toluene용매

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온도
0 °C

실험 절차

41.10 g (0.24 mol) of 5-oxo-5,6,7,8-tetrahydroquinoline-2-carbonitrile were dissolved in 500 ml of toluene, and 35.51 ml (0.25 mol) of 2-(2-methoxyphenyl)ethylamine and 4.54 g (0.024 mol) of p-toluenesulphonic acid monohydrate were added. The reaction solution was then stirred under reflux for 5 hours (using a water separator). Subsequently, the reaction solution was evaporated to dryness and the residue was taken up in 500 ml of ethanol (anhydrous) and, with stirring, cooled to 0° C. A little at a time (careful: reaction mixture foams), 18.06 g (0.48 mol) of sodium borohydride were then added to the reaction solution, and the mixture was stirred overnight. Subsequently, the reaction mixture was concentrated on a rotary evaporator to about 100 ml, and 300 ml of water and 300 ml of ethyl acetate were added. The phases were separated and the aqueous phase was extracted twice with in each case 150 ml of ethyl acetate. The combined organic phases were washed twice with in each case 250 ml of saturated sodium chloride solution, dried over sodium sulphate, filtered and concentrated to a volume of about 150 ml on a rotary evaporator. The solution obtained in this manner was applied to 50 g of silica gel and purified by column chromatography on silica gel (80 g cartridge; flow rate: 75 ml/min; mobile phase: petroleum ether/ethyl acetate 85:15→50:50 over 45 min) This gave 39.03 g (0.10 mol, content 80%, 43% of theory) of the target compound.

후처리

  1. temperatureunder reflux for 5 hours (
  2. customSubsequently, the reaction solution was evaporated to dryness
  3. stirringwith stirring
  4. additionwere then added to the reaction solution
  5. stirringthe mixture was stirred overnight
  6. concentrationSubsequently, the reaction mixture was concentrated on a rotary evaporator to about 100 ml, and 300 ml of water and 300 ml of ethyl acetate
  7. additionwere added
  8. customThe phases were separated
  9. extractionthe aqueous phase was extracted twice with in each case 150 ml of ethyl acetate
  10. washThe combined organic phases were washed twice with in each case 250 ml of saturated sodium chloride solution
  11. dry with materialdried over sodium sulphate
  12. filtrationfiltered
  13. concentrationconcentrated to a volume of about 150 ml on a rotary evaporator
  14. customThe solution obtained in this manner
  15. custompurified by column chromatography on silica gel (80 g cartridge; flow rate: 75 ml/min; mobile phase: petroleum ether/ethyl acetate 85:15→50:50 over 45 min) This gave 39.03 g (0.10 mol, content 80%, 43% of theory) of the target compound

출처 및 근거

ORD 기록
ord-1326c1cf09f64f69b982a793d0f2bde5
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08981104B2

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