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Dichloromethane → HCID 22493592、化合物

HRID 1263460
ノート
印刷プレビュー

反応式

HRID 1263460 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

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

生成物 1

HCID 22493592HCID 22493592、化合物

試薬・触媒・溶媒 1

HCID 14284
4-(Dimethylamino)pyridine
触媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a4e71f244af840219cf2e0809a969fdb
出典データセット
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06541474B2

反応ノート

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