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Ethyl Acetate → N-(2-(1,1-dioxido-4-thiomorpholinyl)ethyl)-N-(2-methoxyethyl)-2-nitrobenzenesulfonamide

HRID 85563
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HRID 85563 반응식
[O:1]=[S:2]1(=[O:23])[CH2:7][CH2:6][N:5]([CH2:8][CH2:9][NH:10][S:11]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[N+:20]([O-:22])=[O:21])(=[O:13])=[O:12])[CH2:4][CH2:3]1.C(=O)([O-])[O-].[Cs+].[Cs+].Br[CH2:31][CH2:32][O:33][CH3:34].C(OCC)(=O)C>CN(C=O)C.O>[O:23]=[S:2]1(=[O:1])[CH2:7][CH2:6][N:5]([CH2:8][CH2:9][N:10]([CH2:31][CH2:32][O:33][CH3:34])[S:11]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[N+:20]([O-:22])=[O:21])(=[O:12])=[O:13])[CH2:4][CH2:3]1
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참가 물질

7

반응물 4

HCID 8857Ethyl AcetateHCID 10796Cesium carbonate2회HCID 809722-Bromoethyl methyl ether2회HCID 68358008N-(2-(1,1-dioxido-4-thiomorpholinyl)ethyl)-2-nitrobenzenesulfonamide

생성물 1

HCID 68358010N-(2-(1,1-dioxido-4-thiomorpholinyl)ethyl)-N-(2-methoxyethyl)-2-nitrobenzenesulfonamide수율 105%

시약·촉매·용매

2
HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

N-(2-(1,1-dioxido-4-thiomorpholinyl)ethyl)-2-nitrobenzenesulfonamide (0.400 g, 1.10 mmol) was combined with cesium carbonate (0.538 g, 1.65 mmol) in DMF (5 mL). The slurry was stirred at rt for 30 min, then to it was added 1-bromo-2-methoxyethane (0.306 g, 2.20 mmol). The resulting mixture was stirred at rt for 72 h. LCMS indicated incomplete conversion, so additional 1-bromo-2-methoxyethane (0.306 g, 2.20 mmol) and cesium carbonate (0.538 g, 1.65 mmol) were added and the mixture was heated to 70° C. for 1 h. Dilution with ethyl acetate (60 mL) and water (40 mL) followed by shaking gave a separation of phases. The organic phase was isolated, washed with water (2×30 mL) and brine (25 mL), dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo to a residue. Purification by silica gel chromatography (gradient 100% DCM to 60:1 DCM:MeOH) gave the title compound as a yellow oil (0.486 g, 105% yield). LCMS: m/z 422 (M+H+), retention time 1.35 min (method 11). 1H NMR (500 MHz, CHLOROFORM-d) δ ppm 2.72 (t, J=6.41 Hz, 2H) 3.01 (s, 8H) 3.21 (s, 3H) 3.39-3.52 (m, 6H) 7.62-7.66 (m, 1H) 7.66-7.74 (m, J=7.48, 7.32, 7.32, 7.32, 1.68 Hz, 2H) 8.01 (dd, J=7.78, 1.68 Hz, 1H).

후처리

  1. stirringThe resulting mixture was stirred at rt for 72 h
  2. additionwere added
  3. temperaturethe mixture was heated to 70° C. for 1 h
  4. stirringby shaking
  5. customgave
  6. customa separation of phases
  7. customThe organic phase was isolated
  8. washwashed with water (2×30 mL) and brine (25 mL)
  9. dry with materialdried over anhydrous magnesium sulfate
  10. filtrationfiltered
  11. concentrationconcentrated in vacuo to a residue
  12. customPurification by silica gel chromatography (gradient 100% DCM to 60:1 DCM:MeOH)

출처 및 근거

ORD 기록
ord-32e1d8b62175412da2d15c3de16e4531
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08846647B2

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