Ammonium Chloride → HCID 67482127, 화합물

HRID 1517272노트

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HRID 1517272 반응식
ClC1C(F)=NC=C(OCCC2OCCO2)C=1.CC(C)([O-])C.[K+].[CH3:23][N:24]1[CH:28]=[CH:27][C:26]([NH:29][C:30]2[C:39]3[C:34](=[CH:35][CH:36]=[C:37](O)[CH:38]=3)[N:33]=[CH:32][N:31]=2)=[N:25]1.[Cl-].[NH4+]>CN(C)C(=O)C>[CH3:23][N:24]1[CH:28]=[CH:27][C:26]([NH:29][C:30]2[C:39]3[C:34](=[CH:35][CH:36]=[CH:37][CH:38]=3)[N:33]=[CH:32][N:31]=2)=[N:25]1

참가 물질

6

반응물 4

HCID 25517Ammonium ChlorideHCID 231603824-[(1-Methyl-1H-pyrazol-3-yl)amino]quinazolin-6-olHCID 23665647Potassium tert-butoxideHCID 684276893-Chloro-5-[2-(1,3-dioxolan-2-yl)ethoxy]-2-fluoropyridine

생성물 1

HCID 67482127HCID 67482127, 화합물수율 151.2%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

3-Chloro-5-[2-(1,3-dioxolan-2-yl)ethoxy]-2-fluoropyridine (4.6 g, 18.4 mmol) and potassium tert-butoxide (2.6 g, 23 mmol) were added to an N,N-dimethylacetamide suspension (5 ml) of 4-[(1-methyl-1H-pyrazol-3-yl)amino]quinazolin-6-ol (2.2 g, 9.1 mmol), and reacted at 200° C. for 2 hours, using microwaves. The reaction solution was cooled to room temperature, aqueous saturated ammonium chloride solution was added, and extracted with ethyl acetate. The organic layer was washed with water and saturated saline water, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=75:25) to obtain 6-03-chloro-5-{[2-(1,3-dioxolan-2-yl)ethoxy]pyridin-2-yl}oxy)-N-(1-methyl-1H-pyrazol-3-yl)quinazoline-4-amine (3.1 g, yield: 73%) as a yellow solid.

후처리

  1. customreacted at 200° C. for 2 hours
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with water and saturated saline water
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=75:25)

출처 및 근거

ORD 기록
ord-f8786d757a4242bcaea4ccb279abf973
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08232284B2

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