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Triethylamine → 3-[4-(2-Fluoro-4-nitrophenoxy)pyridin-2-yl]-1-methyl-1-(1-methylpiperidin-4-yl)urea

HRID 492671
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HRID 492671 반응식
[F:1][C:2]1[CH:15]=[C:14]([N+:16]([O-:18])=[O:17])[CH:13]=[CH:12][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]([NH2:11])[CH:6]=1.[CH2:19]([N:21]([CH2:24][CH3:25])[CH2:22][CH3:23])C.ClC([O:29][C:30]1C=CC=CC=1)=O.[CH3:36][NH:37][CH:38]1CCN(C)CC1>O1CCCC1.CN(C)C=O>[F:1][C:2]1[CH:15]=[C:14]([N+:16]([O-:18])=[O:17])[CH:13]=[CH:12][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]([NH:11][C:30](=[O:29])[N:37]([CH3:38])[CH:36]2[CH2:25][CH2:24][N:21]([CH3:19])[CH2:22][CH2:23]2)[CH:6]=1
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참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 15891Phenyl chloroformateHCID 5663231-Methyl-4-(methylamino)piperidineHCID 231531982-Amino-4-(2-fluoro-4-nitrophenoxy)pyridine

생성물 1

HCID 231533483-[4-(2-Fluoro-4-nitrophenoxy)pyridin-2-yl]-1-methyl-1-(1-methylpiperidin-4-yl)urea수율 75.5%

시약·촉매·용매 2

HCID 6228
Dimethylformamide
용매
HCID 8028Tetrahydrofuran용매

실험 절차

4-(2-Fluoro-4-nitrophenoxy)pyridin-2-ylamine (200 mg) was dissolved in tetrahydrofuran (8 ml) under a nitrogen atmosphere, and then triethylamine (0.336 ml) and phenyl chloroformate (0.302 ml) were added dropwise thereto at room temperature, followed by stirring for 30 min. The reaction mixture was concentrated under a reduced pressure to give a residue, which was dissolved in N,N-dimethylformamide (5 ml), and then N-methyl-N-(1-methylpiperidin-4-yl)amine (0.467 ml) was added thereto at room temperature, followed by stirring for 4 hrs. The reaction mixture was partitioned between ethyl acetate and a saturated aqueous solution of ammonium chloride. The organic layer was washed with a saturated aqueous solution of ammonium chloride, water and brine in this order, and dried over anhydrous sodium sulfate. The solvent was evaporated under a reduced pressure to give a residue, which was purified by silica gel column chromatography (Fuji Silysia NH, eluent; ethyl acetate). The resultant fractions were concentrated under a reduced pressure, and dried in vacuum to provide the titled compound (245 mg, 75.5%) as a yellow solid.

후처리

  1. customat room temperature
  2. concentrationThe reaction mixture was concentrated under a reduced pressure
  3. customto give a residue, which
  4. customat room temperature
  5. stirringby stirring for 4 hrs
  6. customThe reaction mixture was partitioned between ethyl acetate
  7. washThe organic layer was washed with a saturated aqueous solution of ammonium chloride, water and brine in this order
  8. dry with materialdried over anhydrous sodium sulfate
  9. customThe solvent was evaporated under a reduced pressure
  10. customto give a residue, which
  11. customwas purified by silica gel column chromatography (Fuji Silysia NH, eluent; ethyl acetate)
  12. concentrationThe resultant fractions were concentrated under a reduced pressure
  13. customdried in vacuum

출처 및 근거

ORD 기록
ord-2fd5762db30a49159984f08cbfb04a69
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07531532B2

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