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1,2-Dichloroethane → methyl 7-(benzyloxy)-2-bromo-5H-pyrido[3,2-b]indole-4-carboxylate

HRID 2410758
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HRID 2410758 반응식
ClCCCl.[N:5]([C:8]1[C:17]([C:18]2[CH:23]=[CH:22][C:21]([O:24][CH2:25][C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)=[CH:20][CH:19]=2)=[N:16][C:15]([Br:32])=[CH:14][C:9]=1[C:10]([O:12][CH3:13])=[O:11])=[N+]=[N-]>C(Cl)Cl.CCCCCCCC(O)=O.CCCCCCCC(O)=O.CCCCCCCC(O)=O.CCCCCCCC(O)=O.[Rh].[Rh]>[CH2:25]([O:24][C:21]1[CH:20]=[CH:19][C:18]2[C:17]3[N:16]=[C:15]([Br:32])[CH:14]=[C:9]([C:10]([O:12][CH3:13])=[O:11])[C:8]=3[NH:5][C:23]=2[CH:22]=1)[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1
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참가 물질

5

반응물 2

HCID 111,2-DichloroethaneHCID 86663025Methyl 3-azido-2-(4-(benzyloxy)phenyl)-6-bromoisonicotinate

생성물 1

HCID 86663026methyl 7-(benzyloxy)-2-bromo-5H-pyrido[3,2-b]indole-4-carboxylate수율 81%

시약·촉매·용매 2

HCID 6099591Rhodium(II) Octanoate Dimer촉매HCID 6344Dichloromethane용매

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온도
60 °C

실험 절차

1,2-Dichloroethane (3.5 mL) was added to a mixture of methyl 3-azido-2-(4-(benzyloxy)phenyl)-6-bromoisonicotinate (2.28 g, 5.19 mmol), rhodium octanoate dimer (0.101 g, 0.130 mmol) and crushed 4 A° molecular sieves (2.2 gm). This was heated at 60° C. for 6 hr. The reaction was diluted with a mixture of DCM:MeOH=3:1 and filtered. The collected solid was washed with additional DCM:MeOH mixture to dissolve any remaining product. The solvent was removed from the filtrate and the residue was suspended in MeOH. The product was collected by filtration and washed with a little MeOH to leave methyl 7-(benzyloxy)-2-bromo-5H-pyrido[3,2-b]indole-4-carboxylate (1.72 g, 4.18 mmol, 81% yield) as a yellow solid. MS (ESI) m/z 412.9 (M+H). 1H NMR (400 MHz, chloroform-d) δ ppm 9.45 (1H, br. s.), 8.22 (1H, d, J=8.81 Hz), 7.87 (1H, s), 7.43-7.50 (2H, m), 7.37-7.44 (2H, m), 7.30-7.37 (1H, m), 6.96-7.06 (2H, m), 5.18 (2H, s), 4.04 (3H, s).

후처리

  1. customcrushed 4 A° molecular sieves (2.2 gm)
  2. filtrationMeOH=3:1 and filtered
  3. washThe collected solid was washed with additional DCM
  4. dissolutionMeOH mixture to dissolve any remaining product
  5. customThe solvent was removed from the filtrate
  6. filtrationThe product was collected by filtration
  7. washwashed with a little MeOH

출처 및 근거

ORD 기록
ord-6a3c144ace92454492455989d555fbcc
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08815840B2

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