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2,6-Lutidine → N-[1-({2-Chloro-4-[(phenylmethyl)oxy]phenyl}methyl)-1H-pyrazol-3-yl]-2,6-difluorobenzamide

HRID 1946370
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HRID 1946370 반응식
[F:1][C:2]1[CH:15]=[CH:14][CH:13]=[C:12]([F:16])[C:3]=1[C:4]([NH:6][C:7]1[CH:11]=[CH:10][NH:9][N:8]=1)=[O:5].Br[CH2:18][C:19]1[CH:24]=[CH:23][C:22]([O:25][CH2:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)=[CH:21][C:20]=1[Cl:33].N1C(C)=CC=CC=1C>CN1C(=O)CCC1>[Cl:33][C:20]1[CH:21]=[C:22]([O:25][CH2:26][C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)[CH:23]=[CH:24][C:19]=1[CH2:18][N:9]1[CH:10]=[CH:11][C:7]([NH:6][C:4](=[O:5])[C:3]2[C:12]([F:16])=[CH:13][CH:14]=[CH:15][C:2]=2[F:1])=[N:8]1
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참가 물질

5

반응물 3

HCID 79372,6-LutidineHCID 667704731-(Bromomethyl)-2-chloro-4-[(phenylmethyl)oxy]benzeneHCID 178522346HCID 178522346, 화합물2회

생성물 1

HCID 59547945N-[1-({2-Chloro-4-[(phenylmethyl)oxy]phenyl}methyl)-1H-pyrazol-3-yl]-2,6-difluorobenzamide

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

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온도
160 °C

실험 절차

To a solution of 2,6-difluoro-N-(1H-pyrazol-3-yl)benzamide (for a preparation see Intermediate 9)(0.961 g, 4.31 mmol) and 1-(bromomethyl)-2-chloro-4-[(phenylmethyl)oxy]benzene (1.21 g, 3.88 mmol) in anhydrous NMP (15 ml) was added 2,6-lutidine (0.5 ml, 4.29 mmol, Aldrich). The reaction vessel (20 ml) was sealed and heated in Biotage Initiator microwave to 160° C. for 30 min. After cooling the reaction mixture was partitioned between saturated aqueous sodium hydrogen carbonate (120 ml) and ethyl acetate (100 ml). The phases were separated and the aqueous phase extracted with ethyl acetate (50 ml). The combined organic extracts were washed with saturated aqueous sodium hydrogen carbonate (50 ml), dried (MgSO4), filtered and the solvent removed in vacuo to leave a red oil (2.84 g). The residue was loaded in dichloromethane and purified on silica (100 g×2) using 0-100% ethyl acetate-cyclohexane. The appropriate fractions were combined and evaporated in vacuo to give the title compound as a white solid (0.778 g); LCMS: (System 4) MH+=454, tRET=3.35 min.

후처리

  1. customThe reaction vessel (20 ml) was sealed
  2. temperatureAfter cooling the reaction mixture
  3. customwas partitioned between saturated aqueous sodium hydrogen carbonate (120 ml) and ethyl acetate (100 ml)
  4. customThe phases were separated
  5. extractionthe aqueous phase extracted with ethyl acetate (50 ml)
  6. washThe combined organic extracts were washed with saturated aqueous sodium hydrogen carbonate (50 ml)
  7. dry with materialdried (MgSO4)
  8. filtrationfiltered
  9. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-f2fca628f23147f08d8fd95425e5dffc
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08399436B2

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