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Potassium Iodide → 2-(3-(10,11-dihydro-5H-dibenz[b,f]azepin-5-yl)-1-propyl)-1,2,3,4-tetrahydro-3-isoquinolinecarboxylic acid methyl ester

HRID 1166418
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HRID 1166418 반응식
[CH:1]1[C:11]2[CH2:10][CH2:9][C:8]3[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=3[N:6]([CH2:16][CH2:17][CH2:18]O)[C:5]=2[CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.CS(Cl)(=O)=O.[CH3:32][O:33][C:34]([CH:36]1[CH2:45][C:44]2[C:39](=[CH:40][CH:41]=[CH:42][CH:43]=2)[CH2:38][NH:37]1)=[O:35].C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>ClCCl.O.CN(C)C=O>[CH3:32][O:33][C:34]([CH:36]1[CH2:45][C:44]2[C:39](=[CH:40][CH:41]=[CH:42][CH:43]=2)[CH2:38][N:37]1[CH2:18][CH2:17][CH2:16][N:6]1[C:7]2[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=2[CH2:9][CH2:10][C:11]2[CH:1]=[CH:2][CH:3]=[CH:4][C:5]1=2)=[O:35]
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참가 물질

10

반응물 6

HCID 4875Potassium IodideHCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chlorideHCID 4685119Methyl 1,2,3,4-tetrahydroisoquinoline-3-carboxylateHCID 110214143-(10,11-dihydro-5H-dibenz[b,f]azepin-5-yl)-1-propanol

생성물 1

HCID 54478190
2-(3-(10,11-dihydro-5H-dibenz[b,f]azepin-5-yl)-1-propyl)-1,2,3,4-tetrahydro-3-isoquinolinecarboxylic acid methyl ester
수율 76%

시약·촉매·용매 3

HCID 962Water용매2회HCID 6228Dimethylformamide용매2회HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

To a solution of 3-(10,11-dihydro-5H-dibenz[b,f]azepin-5-yl)-1-propanol (1.05 g, 0.0041 mol, prepared similarly as described in example 2) in dichloromethane (40 ml) at 0° C., triethylamine (1.28 g, 0.013 mol) was added, followed by methanesulfonyl chloride (0.9 ml, 0.012 mol). After stirring for 30 minutes at 0° C., water (50 ml) was added and the phases were separated. The organic layer was washed with brine (20 ml), dried (MgSO4) and concentrated in vacuo. The residue was dissolved in acetonitrile (12 ml), and 1,2,3,4-tetrahydro-3-isoquinolinecarboxylic acid methyl ester (1.13 g, 0.0050 mol), N,N-dimethylformamide (5 ml), potassium carbonate (1.32 g, 0.0096 mol) and potassium iodide (0.30 g, 0.0018 mol) were added. The reaction mixture was heated at 82° C. for 12 h. N,N-Dimethylformamide (5 ml) was added and heating was continued for further 16 h. Water (50 ml) was added and the mixture was extracted with ethyl acetate (3×20 ml). The combined organic extracts were washed with brine (2×20 ml), dried (MgSO4) and concentrated in vacuo. The product was purified by column chromatography on silica gel (80 g) using a gradient of heptane and ethyl acetate (10:0→10:3), affording 1.4 g (76%) of 2-(3-(10,11-dihydro-5H-dibenz[b,f]azepin-5-yl)-1-propyl)-1,2,3,4-tetrahydro-3-isoquinolinecarboxylic acid methyl ester as an oil.

후처리

  1. customat 0° C.
  2. customthe phases were separated
  3. washThe organic layer was washed with brine (20 ml)
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. dissolutionThe residue was dissolved in acetonitrile (12 ml)
  7. temperatureThe reaction mixture was heated at 82° C. for 12 h
  8. temperatureheating
  9. waitwas continued for further 16 h
  10. extractionthe mixture was extracted with ethyl acetate (3×20 ml)
  11. washThe combined organic extracts were washed with brine (2×20 ml)
  12. dry with materialdried (MgSO4)
  13. concentrationconcentrated in vacuo
  14. customThe product was purified by column chromatography on silica gel (80 g)

출처 및 근거

ORD 기록
ord-6ff8adb7e0dd4fefbf085a988136a304
출처 데이터셋
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06613791B1

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