2(1H)-Pyrimidinone, tetrahydro- → HCID 59586732, 화합물

HRID 218529

반응식

HRID 218529 반응식
[NH:1]1[CH2:6][CH2:5][CH2:4][NH:3][C:2]1=[O:7].CC(C)([O-])C.[K+].F[C:15]1[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][C:16]=1[CH:24]([CH3:26])[CH3:25]>CS(C)=O.O>[CH:24]([C:16]1[CH:17]=[C:18]([N+:21]([O-:23])=[O:22])[CH:19]=[CH:20][C:15]=1[N:1]1[CH2:6][CH2:5][CH2:4][NH:3][C:2]1=[O:7])([CH3:26])[CH3:25]

참가 물질

6

반응물 3

HCID 746152(1H)-Pyrimidinone, tetrahydro-HCID 23665647Potassium tert-butoxideHCID 598604881-Fluoro-2-isopropyl-4-nitrobenzene

생성물 1

HCID 59586732HCID 59586732, 화합물

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

실험 절차

347 mg (3.47 mmol) of tetrahydropyrimidinone in 21 ml of DMSO are admixed at RT with 584 mg (5.21 mmol) of potassium tert-butoxide, and the mixture is stirred at RT for 45 min. 700 mg (3.82 mmol) of 1-fluoro-2-isopropyl-4-nitrobenzene are added and the mixture is stirred at 60° C. After 18 h, it is cooled and diluted with 250 ml of water. It is extracted three times with ethyl acetate and the combined organic phases are dried over sodium sulfate. After filtration, the solvents are removed under reduced pressure and the residue is purified by chromatography on silica gel (1:5→1:10 cyclohexane/ethyl acetate). This affords 140 mg (14% of theory) of the desired compound.

후처리

  1. stirringthe mixture is stirred at 60° C
  2. waitAfter 18 h
  3. temperatureit is cooled
  4. extractionIt is extracted three times with ethyl acetate
  5. dry with materialthe combined organic phases are dried over sodium sulfate
  6. filtrationAfter filtration
  7. customthe solvents are removed under reduced pressure
  8. customthe residue is purified by chromatography on silica gel (1:5→1:10 cyclohexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-8a186f2eb15b422db9d30e34aaf3fc64
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08198267B2

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