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Potassium Carbonate → HCID 67337246, 화합물

HRID 1673034
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HRID 1673034 반응식
Cl[C:2]1[CH:3]=[C:4]([C:24]2[CH:29]=[CH:28][CH:27]=[C:26]([S:30]([CH3:33])(=[O:32])=[O:31])[CH:25]=2)[CH:5]=[CH:6][C:7]=1[N:8]1[CH:12]=[C:11]([C:13](O)=[O:14])[N:10]=[C:9]1[CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[Cl:23].BrC1C=CC([N:41]2C=C(C(O)=O)[N:43]=[C:42]2[C:49]2C=CC=CC=2Cl)=C(Cl)C=1.C(Cl)(=O)C(Cl)=O.C(=NO)(N)C.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.CCOC(C)=O.C1(C)C(C)=CC=CC=1.C(Cl)(Cl)Cl>[CH3:33][S:30]([C:26]1[CH:25]=[C:24]([C:4]2[CH:5]=[CH:6][C:7]([N:8]3[CH:12]=[C:11]([C:13]4[O:14][N:43]=[C:42]([CH3:49])[N:41]=4)[N:10]=[C:9]3[CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[Cl:23])=[CH:2][CH:3]=2)[CH:29]=[CH:28][CH:27]=1)(=[O:31])=[O:32]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 5

HCID 11430Potassium CarbonateHCID 30926N-HydroxyacetamidineHCID 65578Oxalyl chlorideHCID 59240289HCID 59240289, 화합물HCID 67337145HCID 67337145, 화합물

생성물 1

HCID 67337246HCID 67337246, 화합물수율 31%

시약·촉매·용매 4

HCID 6228Dimethylformamide촉매HCID 6212Chloroform용매HCID 7237O-Xylene용매HCID 8857Ethyl Acetate용매

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온도
0 °C

실험 절차

To a 100 mL round bottom flask was added 1-(3-Chloro-3′-methanesulfonylbiphenyl-4-yl)-2-(2-chlorobenzyl)-1H-imidazole-4-carboxylic acid, obtained in a manner similar to that described for 1-(4-Bromo-2-chloro-phenyl)-2-(2-chlorophenyl)-1H-imidazole-4-carboxylic acid in Example BB1 (350 mg, 707 μmol) and anhydrous CHCl3 (15 mL). The reaction solution was cooled to 0° C. prior to addition of oxalyl chloride (310 μL, 3.54 mmol) and 1 drop of anhydrous DMF. The reaction solution was allowed to stir warming to room temperature over 1.5 h. The solution was concentrated in vacuo and the residue was dissolved in anhydrous 1,4-dioxane (20 mL). To the reaction flask was added acetamide oxime (104 mg, 1.41 mmol) and K2CO3 (293 mg, 2.12 mmol). The mixture was stirred at room temperature for 1 hr prior to addition of xylene (43 mL) and raising the reaction temperature to reflux for 16 hrs. The reaction solution was diluted with EtOAc (100 mL) and washed with sat aq. NH4Cl (150 mL×2). The organic phase was dried over Na2SO4, filtered, concentrated in vacuo, and chromatographed through a 25 g SiO2 column using a 100% hexane to 100% EtOAc gradient to yield 115 mg (31% yield) of title compound. MS (ESI) 533.3, 535.3 [M+H]+; 1H NMR (400 MHz, DMSO-d6) δ 8.16 (s, 1H), 8.06 (s, 1H), 7.97 (d, J=7.6 Hz, 1H), 7.91 (d, J=7.6 Hz, 1H), 7.76 (t, J=7.6 Hz, 1H), 7.50 (d, J=8.4 Hz, 2H), 7.26 (dd, J=7.8 Hz, J2=1 Hz, 1H), 7.12 (d, J=8.4 Hz, 2H), 7.09 (m, 1H), 7.02 (dd, J=7.8 Hz, J2=1 Hz, 1H), 6.95 (t, J=8 Hz, 1H), 3.32 (s, 3H), 2.39 (s, 3H), 1.79 (s, 3H).

후처리

  1. customobtained in a manner similar to
  2. temperaturewarming to room temperature over 1.5 h
  3. concentrationThe solution was concentrated in vacuo
  4. dissolutionthe residue was dissolved in anhydrous 1,4-dioxane (20 mL)
  5. stirringThe mixture was stirred at room temperature for 1 hr
  6. temperatureraising the reaction temperature
  7. temperatureto reflux for 16 hrs
  8. washwashed
  9. dry with materialThe organic phase was dried over Na2SO4
  10. filtrationfiltered
  11. concentrationconcentrated in vacuo
  12. customchromatographed through a 25 g SiO2 column

출처 및 근거

ORD 기록
ord-e589fbf5330945b098d56ce37d5d6157
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07998995B2

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