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Pyridine → HCID 58713644, 화합물

HRID 475513
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HRID 475513 반응식
[C:1]([O:5][C:6]([C:8]1[C:12]2[CH2:13][C:14]([O:16][CH2:17][CH3:18])=[CH:15][C:11]=2[NH:10][N:9]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].N1C=CC=CC=1.[C:25]1([CH3:35])[CH:30]=[CH:29][C:28]([S:31](Cl)(=[O:33])=[O:32])=[CH:27][CH:26]=1>C(Cl)Cl>[C:1]([O:5][C:6]([C:8]1[C:12]2[CH2:13][C:14]([O:16][CH2:17][CH3:18])=[CH:15][C:11]=2[N:10]([S:31]([C:28]2[CH:29]=[CH:30][C:25]([CH3:35])=[CH:26][CH:27]=2)(=[O:33])=[O:32])[N:9]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
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참가 물질

5

반응물 3

HCID 1049PyridineHCID 73974-Toluenesulfonyl chlorideHCID 58713648HCID 58713648, 화합물

생성물 1

HCID 58713644HCID 58713644, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of the pyrazole intermediate from step A (275 mg, 1.1 mmol) above in CH2Cl2 (5 mL) was added pyridine (178 μL, 2.2 mmol) and p-toluene sulfonyl chloride (230 mg, 1.21 mmol). After stirring the resulting reaction mixture at room temperature for 3 hours it was diluted with CH2Cl2, washed with 1N HCl, saturated NaHCO3, dried over anhydrous Na2SO4, filtered and concentrated in vacuo. The residue was purified by flash chromatography (SiO2) using 10% ethyl acetate-hexanes.

후처리

  1. customthe resulting reaction mixture at room temperature for 3 hours it
  2. washwashed with 1N HCl, saturated NaHCO3
  3. dry with materialdried over anhydrous Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by flash chromatography (SiO2)

출처 및 근거

ORD 기록
ord-ab3d9ed445174e99b556fc7fdccda065
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08637555B2

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