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Potassium Iodide → HCID 10157486, 화합물

HRID 966474
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HRID 966474 반응식
[CH2:1]([O:8][C:9]([C:11]1[C:19]2[C:14](=[CH:15][CH:16]=[C:17]([O:20][CH2:21][CH2:22]Cl)[CH:18]=2)[N:13]([CH3:24])[C:12]=1[CH3:25])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+].[CH2:34]([NH:36][CH2:37][CH3:38])[CH3:35].[K+].[Br-]>CN(C=O)C.O.CC#N>[CH2:1]([O:8][C:9]([C:11]1[C:19]2[C:14](=[CH:15][CH:16]=[C:17]([O:20][CH2:21][CH2:22][N:36]([CH2:37][CH3:38])[CH2:34][CH3:35])[CH:18]=2)[N:13]([CH3:24])[C:12]=1[CH3:25])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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참가 물질

9

반응물 5

HCID 4875Potassium IodideHCID 8021Diethylamine2회HCID 11430Potassium CarbonateHCID 253877Potassium BromideHCID 23393870HCID 23393870, 화합물

생성물 1

HCID 10157486HCID 10157486, 화합물

시약·촉매·용매 3

HCID 962
Water
용매
HCID 6228Dimethylformamide용매
HCID 6342Acetonitrile용매

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온도
100 °C

실험 절차

To a mixture of 1-methyl-5-(2-chloro-ethoxy)-2-methyl-1H-indole-3-carboxylic acid benzyl ester (0.576 mmol, 0.206 g, Example 8, Step A) in 5.76 mL of DMF was added potassium carbonate (0.576 mmol, 0.080 g), potassium iodide (0.0576 mmol, 0.010 g), and diethylamine (2.30 mmol, 0.238 mL, Aldrich). The mixture was heated at 100° C. for 20 hours, an additional 2.30 mmol of diethylamine was added and heating was continued for 21 hours. The solution was cooled to room temperature, diluted with water (10 mL), and extracted with ethyl acetate (4×15 mL). The combined extracts were washed with water (10 mL), saturated aqueous NaCl (10 mL), dried over MgSO4, and concentrated to a brown oil (0.234 g). The product was purified by silica gel flash column chromatography (5-10% MeOH/CH2Cl2) to give a tan solid (0.114 g, 50/o): mp 73-74° C.; IR (KBr) 2968, 2918, 1692, 1186, 1101 cm−1; 1HNMR (400 MHz, DMSO-d6) δ 0.92 (t, J=7.08 Hz, 6H, N(CH2CH3)2), 2.46-2.51 (m, 4H, 2 NCH2), 2.66 (s, 3H, ArCH3), 2.68-2.73 (m, 2H, NCH2), 3.65 (s, 3H, NCH3), 3.85 (t, J=6.11 Hz, 2H, CH2OAr), 5.28 (s, 2H, CO2CH2Ph), 6.75 (dd, J=8.79, 2.44 Hz, 1H, ArH), 7.28-7.32 (m, 1H, ArH), 7.35-7.39 (m, 4H, ArH), 7.46 (d, J=7.57 Hz, 2H, ArH); MS(APCI+): m/z 395.1 (M+1). HPLC (ALLTECH/ALLTIMA C-18,50:50-2:98H2O/CH3CN+0.05% TFA): retention time=3.617 min, 96.84% purity.

후처리

  1. temperatureheating
  2. temperatureThe solution was cooled to room temperature
  3. extractionextracted with ethyl acetate (4×15 mL)
  4. washThe combined extracts were washed with water (10 mL), saturated aqueous NaCl (10 mL)
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated to a brown oil (0.234 g)
  7. customThe product was purified by silica gel flash column chromatography (5-10% MeOH/CH2Cl2)
  8. customto give a tan solid (0.114 g, 50/o)

출처 및 근거

ORD 기록
ord-61289bda7cc94de69cf4e1c6ad1eb929
출처 데이터셋
uspto-grants-2005_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06951848B2

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