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Potassium Carbonate → Tert-butyl 3-(4,6-bistrifluoromethylpyridin-2-yl)propylcarbamate

HRID 444793
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HRID 444793 반응식
[CH2:1]([NH:4][C:5](=[O:11])[O:6][C:7]([CH3:10])([CH3:9])[CH3:8])[CH:2]=[CH2:3].C12BC(CCC1)CCC2.Br[C:22]1[CH:27]=[C:26]([C:28]([F:31])([F:30])[F:29])[CH:25]=[C:24]([C:32]([F:35])([F:34])[F:33])[N:23]=1.C([O-])([O-])=O.[K+].[K+]>C1COCC1.CN(C=O)C.CC([O-])=O.CC([O-])=O.[Pd+2].C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.[Fe+2].O>[F:31][C:28]([F:29])([F:30])[C:26]1[CH:25]=[C:24]([C:32]([F:33])([F:34])[F:35])[N:23]=[C:22]([CH2:3][CH2:2][CH2:1][NH:4][C:5](=[O:11])[O:6][C:7]([CH3:10])([CH3:9])[CH3:8])[CH:27]=1
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참가 물질

10

반응물 4

HCID 11430Potassium CarbonateHCID 789669-Borabicyclo(3.3.1)nonaneHCID 4067274tert-butyl N-(prop-2-en-1-yl)carbamateHCID 85875928Pyridine, 2-bromo-4,6-bis(trifluoromethyl)-

생성물 1

HCID 86650694Tert-butyl 3-(4,6-bistrifluoromethylpyridin-2-yl)propylcarbamate수율 74%

시약·촉매·용매 5

HCID 167845
palladium(II) acetate
촉매
HCID 635956Ferrocene-1,1'-bis-(diphenylphosphine)촉매
HCID 962Water용매
HCID 6228Dimethylformamide용매
HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of tert-butyl allylcarbamate (1.95 g, 12.4 mmol) in THF (12 mL), 0.5 mol/L 9-borabicyclo[3.3.1]nonane (29.8 mL, 14.9 mmol) was added under argon atmosphere at room temperature. After stirred at room temperature for 4 h, a solution of 2-bromo-4,6-bistrifluoromethylpyridine (3.65 g, 12.4 mmol) in DMF (12 mL), Pd(OAc)2 (278 mg, 1.24 mmol), DPPF (859 mg, 1.55 mmol) and K2CO3 (2.92 g, 21.1 mmol) were added to the reaction mixture and stirred at room temperature for 7 h. To the reaction mixture, water was added and the crude product was extracted with EtOAc, washed with brine, dried over NaSO4 and the solvent was removed in vacuo. The crude product was purified by column chromatography (Hexane:EtOAc 10:1→2:1) to yield tert-butyl 3-(4,6-bistrifluoromethylpyridin-2-yl)propylcarbamate (3.41 g, 74%) as a colorless solid. 1H NMR (CDCl3, 400 MHz) δ 1.44 (9H, s), 1.96-2.03 (2H, m), 2.98-3.02 (2H, m), 3.20-3.25 (2H, m), 4.71 (1H, brs), 7.59 (1H, s), 7.72 (1H, s). CIMS (+) 373 [M+H]+.

후처리

  1. stirringstirred at room temperature for 7 h
  2. extractionthe crude product was extracted with EtOAc
  3. washwashed with brine
  4. dry with materialdried over NaSO4
  5. customthe solvent was removed in vacuo
  6. customThe crude product was purified by column chromatography (Hexane:EtOAc 10:1→2:1)

출처 및 근거

ORD 기록
ord-a2417668deaa487fb23f75a774839b97
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08476261B2

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