Lawesson's reagent → HCID 86650591, 화합물

HRID 1257382노트

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HRID 1257382 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:10]=1)[C:5]([NH2:7])=O.COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:24]2)=CC=1.C(=O)([O-])O.[Na+]>O1CCCC1>[Br:1][C:2]1[CH:3]=[C:4]([C:5](=[S:24])[NH2:7])[CH:8]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:10]=1

참가 물질

5

반응물 3

HCID 87949Lawesson's reagentHCID 516892Sodium BicarbonateHCID 593165253-Bromo-5-(trifluoromethyl)benzamide

생성물 1

HCID 86650591HCID 86650591, 화합물수율 83%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
80 °C

실험 절차

To a solution (30 mL) of the compound (3.7 g, 14 mmol) obtained in Example 77a in tetrahydrofuran was added 2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane 2,4-disulfide (5.5 g, 14 mmol), and the mixture was stirred at 80° C. for 5 hr. Saturated aqueous sodium hydrogen carbonate was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The obtained organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The resulting crude title compound was recrystallized (hexane-ethyl acetate) to give the title compound (3.2 g, 83%) as pale-yellow crystals.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe obtained organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customThe resulting crude title compound was recrystallized (hexane-ethyl acetate)

출처 및 근거

ORD 기록
ord-2e85c61dec094b3e86af6cdf10b804f9
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08461348B2

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