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Hydrochloric Acid → 6-chloro-1-(2,4-dichlorobenzoyl)-2,3-dihydro-3-methyl-4(1H)-quinolinone

HRID 1904660
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HRID 1904660 반응식
C(NC(C)C)(C)C.C([Li])CCC.CC(C)=O.[C:17](=[O:19])=O.[Cl:20][C:21]1[CH:22]=[C:23]2[C:28](=[CH:29][CH:30]=1)[N:27]([C:31](=[O:40])[C:32]1[CH:37]=[CH:36][C:35]([Cl:38])=[CH:34][C:33]=1[Cl:39])[CH2:26][CH2:25][C:24]2=O.CI.Cl>O1CCCC1.C(OCC)(=O)C.O.CCCCCC>[Cl:20][C:21]1[CH:30]=[C:29]2[C:28](=[CH:23][CH:22]=1)[N:27]([C:31](=[O:40])[C:32]1[CH:37]=[CH:36][C:35]([Cl:38])=[CH:34][C:33]=1[Cl:39])[CH2:26][CH:25]([CH3:24])[C:17]2=[O:19]
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참가 물질

11

반응물 6

HCID 313Hydrochloric AcidHCID 6328Methyl iodideHCID 7912DiisopropylamineHCID 10522118HCID 10522118, 화합물HCID 18522661Acetone cardiceHCID 178418339Butyllithium

생성물 1

HCID 14501493
6-chloro-1-(2,4-dichlorobenzoyl)-2,3-dihydro-3-methyl-4(1H)-quinolinone

시약·촉매·용매 4

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회HCID 8058Hexane용매HCID 8857Ethyl Acetate용매

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온도
0 °C

실험 절차

To a cooled (-20° C. to -15° C.) solution of diisopropylamine (4.7 g) in anhydrous tetrahydrofuran (100 ml) was added dropwise n-hexane solution (29 ml) of 1.6 N butyl lithium over a 30-minute period in a nitrogen atmosphere, and stirring was continued for 30 minutes after the mixed solution was returned to 0° C. Then the solution was cooled to -75° C. with acetone-dry ice and 15 g of 6-chloro-1-(2,4dichloro-benzoyl)-2,3-dihydro-4(1H)-quinolinone dissolved in 150 ml of anhydrous tetrahydrofuran was added dropwise over a 1-hour period. The reaction mixture was stirred for another 1 hour at -75° C., and methyl iodide (18 g) was added dropwise with stirring over a 30-minute period. The reaction mixture was then slowly warmed to 0° C. over two hour, and acidified under cooling with 2 N hydrochloric acid to be weakly acidic. The reaction mixture was poured into 300 ml of water, then shaken with ethyl acetate (500 ml). The organic layer was washed once with saturated aqueous NaCl solution (200 ml) and dried over anhydrous sodium aulfate. Ethyl acetate was removed in vacuo and the residue was subjected to silica gel column chromatography using a hexane-ethyl acetate mixture (4: 1) to obtain 6-chloro-1-(2,4-dichlorobenzoyl)-2,3-dihydro-3-methyl-4(1H) -quinolinone (yield 7.8 g) as white crystal.

후처리

  1. customwas returned to 0° C
  2. additionwas added dropwise over a 1-hour period
  3. stirringThe reaction mixture was stirred for another 1 hour at -75° C.
  4. stirringwith stirring over a 30-minute period
  5. washThe organic layer was washed once with saturated aqueous NaCl solution (200 ml)
  6. dry with materialdried over anhydrous sodium aulfate
  7. customEthyl acetate was removed in vacuo

출처 및 근거

ORD 기록
ord-fb69d89175444380962b69ada026a12a
출처 데이터셋
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04839368

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