2(1H)-Pyrimidinone, tetrahydro- → HCID 59586732、化合物

HRID 218529

反応式

HRID 218529 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 59586732HCID 59586732、化合物

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-8a186f2eb15b422db9d30e34aaf3fc64
出典データセット
uspto-grants-2012_06
特許番号
US08198267B2

関連ノート

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