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Dichloromethane → HCID 22493592, 화합물

HRID 986930
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HRID 986930 반응식
N1[C:6]([CH3:7])=[CH:5][CH:4]=[CH:3][C:2]=1[CH3:8].[F:9][C:10]([F:23])([F:22])[S:11]([O:14]S(C(F)(F)F)(=O)=O)(=[O:13])=[O:12].[Cl-].[NH4+:25].[C:26]([O:29][CH2:30]C)(=[O:28])C.CC[CH2:34][CH2:35][CH2:36][CH3:37].Cl[CH2:39]Cl>CN(C)C1C=CN=CC=1>[F:9][C:10]([F:23])([F:22])[S:11]([O:14][C:3]1[C:4]2[C:34](=[C:35]([CH:36]([CH3:37])[CH3:39])[CH:7]=[CH:6][CH:5]=2)[N:25]=[C:8]([C:26]([O:29][CH3:30])=[O:28])[CH:2]=1)(=[O:13])=[O:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 6344DichloromethaneHCID 79372,6-LutidineHCID 25517Ammonium ChlorideHCID 67749Trifluoromethanesulfonic anhydrideHCID 21226206Ethyl acetate hexane

생성물 1

HCID 22493592HCID 22493592, 화합물

시약·촉매·용매 1

HCID 14284
4-(Dimethylamino)pyridine
촉매

실험 절차

In 100 ml of dichloromethane were dissolved 4.2 g of methyl 8-isopropylquinolone-2-carboxylate, 3 ml of 2,6-lutidine and 209 mg of 4-dimethylaminopyridine under a nitrogen gas stream. Trifluoromethanesulfonic anhydride (3.2 ml) was added dropwise to the resulting solution at 0° C., followed by stirring at room temperature for 24 hours. A saturated aqueous solution of ammonium chloride was added to the reaction mixture and the resulting mixture was extracted with dichloromethane. The organic layer was successively washed with water and saturated saline, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue so obtained was subjected to chromatography on a silica gel column (developing solvent: 5% ethyl acetate/n-hexane), whereby 6.3 g of the title compound were obtained in the form of a colorless solid.

후처리

  1. extractionthe resulting mixture was extracted with dichloromethane
  2. washThe organic layer was successively washed with water and saturated saline
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue so obtained

출처 및 근거

ORD 기록
ord-de60dbd62761450b851e4433bf8b163c
출처 데이터셋
uspto-grants-2003_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06630463B2

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