Butyl iodide → HCID 13535694, 화합물

HRID 1583652노트

반응식

HRID 1583652 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][NH:9][C:10]2[CH:11]=[N:12][CH:13]=[N:14][CH:15]=2)=[CH:4][CH:3]=1.[H-].[K+].I[CH2:19][CH2:20][CH2:21][CH3:22]>O1CCCC1>[CH2:19]([N:9]([C:10]1[CH:15]=[N:14][CH:13]=[N:12][CH:11]=1)[CH2:8][C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=1)[CH2:20][CH2:21][CH3:22]

참가 물질

5

반응물 3

HCID 10962Butyl iodideHCID 82127Potassium hydrideHCID 13535693N-[(4-chlorophenyl)methyl]-(5-pyrimidyl)amine

생성물 1

HCID 13535694HCID 13535694, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 2.2 g of N-[(4-chlorophenyl)methyl]-(5-pyrimidyl)amine dissolved in 50 ml of tetrahydrofuran was added 2 g of a 24.6% suspension of potassium hydride in oil. The reaction was allowed to stir at room temperature for approximately 1 hour at which time 2 g of iodobutane was added to the reaction mixture. The mixture was stirred at room temperature overnight and concentrated under reduced pressure. The residue was dissolved in diethyl ether and the organic phase was washed with water, separated and dried over anhydrous magnesium sulfate. Following concentration of the solution under reduced pressure the residue was chromatographed over silica gel. Fractions containing the major component were combined and the solvent was evaporated therefrom to afford N-butyl-N-[(4-chlorophenyl)methyl]-(5-pyrimidyl)amine as a solid. mp=67°-68° C.

후처리

  1. additionwas added to the reaction mixture
  2. concentrationconcentrated under reduced pressure
  3. dissolutionThe residue was dissolved in diethyl ether
  4. washthe organic phase was washed with water
  5. customseparated
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customwas chromatographed over silica gel
  8. additionFractions containing the major component
  9. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-e46af3dc58704366b0afd0bbd0b210fe
출처 데이터셋
uspto-grants-1985_11
특허 번호
US04552960

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