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Water → 1-(4-Chlorobutyl)-4-(trifluoromethyl)pyrimidin-2(1H)-one

HRID 1678081
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HRID 1678081 반응식
[OH:1][C:2]1[N:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[CH:4][N:3]=1.C([O-])([O-])=O.[K+].[K+].Br[CH2:19][CH2:20][CH2:21][CH2:22][Cl:23].O>CN(C)C=O>[Cl:23][CH2:22][CH2:21][CH2:20][CH2:19][N:3]1[CH:4]=[CH:5][C:6]([C:8]([F:11])([F:9])[F:10])=[N:7][C:2]1=[O:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 813641-Bromo-4-chlorobutaneHCID 178517744HCID 178517744, 화합물

생성물 1

HCID 673737351-(4-Chlorobutyl)-4-(trifluoromethyl)pyrimidin-2(1H)-one

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4.6 g (28.3 mmol) of 2-hydroxy-4-trifluoromethylpyrimidine were stirred in 60 ml of N,N-dimethylformamide (DMF) and 3.9 g (28.3 mmol) of K2CO3 at room temperature for 1 hour. Then 4.9 g (28.3 mmol) of 1-bromo-4-chlorobutane were added dropwise, and the reaction mixture was stirred at room temperature for 6 hours. Water was then added to the reaction mixture, and the aqueous mixture was extracted with diethyl ether. The aqueous phase was made alkaline by adding NaOH, and the aqueous phase was extracted with methylene chloride. The organic phase was then dried, the desiccant was removed by filtration, and the solvent was evaporated to dryness in vacuo; yield: 1.7 g.

후처리

  1. extractionthe aqueous mixture was extracted with diethyl ether
  2. additionby adding NaOH
  3. extractionthe aqueous phase was extracted with methylene chloride
  4. customThe organic phase was then dried
  5. customthe desiccant was removed by filtration
  6. customthe solvent was evaporated to dryness in vacuo

출처 및 근거

ORD 기록
ord-be156d9ed4784c38bd6c91c61d3abc48
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08008488B2

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