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Sodium Carbonate → 3-[5-(6-Amino-5-trifluoromethyl-pyridin-3-yl)-imidazo[2,1-b][1,3,4]thiadiazol-2-yl]-benzonitrile

HRID 2409565
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HRID 2409565 반응식
Br[C:2]1[S:6][C:5]2=[N:7][CH:8]=[C:9](I)[N:4]2[N:3]=1.[C:11]([C:13]1[CH:14]=[C:15](B(O)O)[CH:16]=[CH:17][CH:18]=1)#[N:12].C([O-])([O-])=O.[Na+].[Na+].CC1(C)C(C)(C)OB([C:36]2[CH:37]=[C:38]([C:43]([F:46])([F:45])[F:44])[C:39]([NH2:42])=[N:40][CH:41]=2)O1.C([O-])([O-])=O.[K+].[K+]>O1CCOCC1>[NH2:42][C:39]1[N:40]=[CH:41][C:36]([C:9]2[N:4]3[C:5]([S:6][C:2]([C:17]4[CH:18]=[C:13]([CH:14]=[CH:15][CH:16]=4)[C:11]#[N:12])=[N:3]3)=[N:7][CH:8]=2)=[CH:37][C:38]=1[C:43]([F:46])([F:44])[F:45]
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HCID 10340Sodium CarbonateHCID 11430Potassium CarbonateHCID 27343253-Cyanophenylboronic acidHCID 468641035-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)-3-(trifluoromethyl)pyridin-2-amineHCID 662215402-Bromo-5-iodoimidazo[2,1-b][1,3,4]thiadiazole

생성물 1

HCID 66716964
3-[5-(6-Amino-5-trifluoromethyl-pyridin-3-yl)-imidazo[2,1-b][1,3,4]thiadiazol-2-yl]-benzonitrile

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
110 °C

실험 절차

To a mixture of 2-bromo-5-iodoimidazo[2,1-b][1,3,4]thiadiazole (0.150 g, 0.455 mmol), 3-cyanophenylboronic acid (0.477 mmol) and PdCl2(Ph3P)2 (0.064 g) in dioxane (3 mL), an aq. solution of Na2CO3(2 M, 0.9 mL) was added. The reaction mixture was heated at 110° C. for 24 h in a sealed tube. The solvent was evaporated, the residue precipitated with water, and after drying the resulting gum was washed with Et2O. The residue was suspended in dioxane (3 mL), and 5-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-3-trifluoromethyl-pyridin-2-ylamine (1.05 eq), PdCl2(Ph3P)2 (0.2 eq) and a sat. aq. solution of K2CO3 (0.9 mL) were added. The reaction mixture was heated at 100° C. for 16 h and then concentrated to dryness. The residue was washed with water, followed by ethyl ether. The resulting solid was washed with DCM followed by MeOH. The DCM filtrate was evaporated and purified by HPLC to yield the desired product (0.10 g). HPLC-MS: (5-100% B in 8 min, 0.8 mL/min, 50° C.): tR=5.15 min, [M+H]+ m/z 387.1; 1H NMR (300 MHz, DMSO-d6) δ 8.90 (s, 1H), 8.49 (s, 1H), 8.38-8.25 (m, 2H), 8.12 (d, J=7.9 Hz, 1H), 7.92-7.74 (m, 2H), 6.75 (s, 2H) ppm.

후처리

  1. customThe solvent was evaporated
  2. customthe residue precipitated with water
  3. customafter drying the resulting gum
  4. washwas washed with Et2O
  5. temperatureThe reaction mixture was heated at 100° C. for 16 h
  6. concentrationconcentrated to dryness
  7. washThe residue was washed with water
  8. washThe resulting solid was washed with DCM
  9. customThe DCM filtrate was evaporated
  10. custompurified by HPLC

출처 및 근거

ORD 기록
ord-283f867686d0421cbbdb11efb03d89ae
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08815918B2

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