Water → Ethyl 1-cyclopropyl-5-ethinyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylate

HRID 2258123노트

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HRID 2258123 반응식
[CH:1]1([N:4]2[C:13]3[C:8](=[C:9]([C:17]#[C:18][Si](C)(C)C)[C:10]([F:16])=[C:11]([F:15])[C:12]=3[F:14])[C:7](=[O:23])[C:6]([C:24]([O:26][CH2:27][CH3:28])=[O:25])=[CH:5]2)[CH2:3][CH2:2]1.[F-].[K+].C(Cl)(Cl)Cl.O>CN(C)C=O>[CH:1]1([N:4]2[C:13]3[C:8](=[C:9]([C:17]#[CH:18])[C:10]([F:16])=[C:11]([F:15])[C:12]=3[F:14])[C:7](=[O:23])[C:6]([C:24]([O:26][CH2:27][CH3:28])=[O:25])=[CH:5]2)[CH2:3][CH2:2]1

참가 물질

6

반응물 4

HCID 962WaterHCID 6212Chloroform2회HCID 522689Potassium FluorideHCID 22924385Ethyl 1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-5-trimethylsilylethinyl-4-oxo-3-quinolinecarboxylate

생성물 1

HCID 22924399Ethyl 1-cyclopropyl-5-ethinyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylate수율 76.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

1 g of the product of Example E and 0.45 g of potassium fluoride are stirred for 1 hour at room temperature in a mixture of 20 ml of dimethylformamide, 10 ml of chloroform and 1 ml of water. After chloroform has been added, the organic phase is separated off, extracted by shaking with water, dried over sodium sulphate and concentrated. The residue is boiled briefly in 20 ml of methanol. When the mixture has cooled to 0° C., the solid obtained is filtered off with suction and dried. 0.63 g of the title compound is obtained (77% of theory).

후처리

  1. customthe organic phase is separated off
  2. extractionextracted
  3. dry with materialdried over sodium sulphate
  4. concentrationconcentrated
  5. customthe solid obtained
  6. filtrationis filtered off with suction
  7. customdried

출처 및 근거

ORD 기록
ord-154cf26683fe41bb8039c34990ddd31d
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05659038

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