Butyl iodide → HCID 13535694、化合物

HRID 1583652ノート

反応式

HRID 1583652 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 13535694HCID 13535694、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e46af3dc58704366b0afd0bbd0b210fe
出典データセット
uspto-grants-1985_11
特許番号
US04552960

反応ノート

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