N-bromobutanimide → 2-bromo-4-(4-pyridinylmethyl)Benzenamine

HRID 1417245

反応式

HRID 1417245 の反応式
[Br:1]N1C(=O)CCC1=O.[N:9]1[CH:14]=[CH:13][C:12]([CH2:15][C:16]2[CH:22]=[CH:21][C:19]([NH2:20])=[CH:18][CH:17]=2)=[CH:11][CH:10]=1>CN(C)C=O.C(OCC)C>[Br:1][C:18]1[CH:17]=[C:16]([CH2:15][C:12]2[CH:13]=[CH:14][N:9]=[CH:10][CH:11]=2)[CH:22]=[CH:21][C:19]=1[NH2:20]

参加物

5

反応物 2

HCID 67184N-bromobutanimideHCID 3071584-[(Pyridin-4-yl)methyl]aniline

生成物 1

HCID 218656452-bromo-4-(4-pyridinylmethyl)Benzenamine

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒2 回

実験手順

A solution of 18.34 g (0.103 mol) of N-bromosuccinimide in 60 ml of dimethylformamide is added dropwise, shielded from light, to a solution of 20 g (0.1084 mol) of 4-(4-pyridylmethyl)aniline in 180 ml of dimethylformamide. After 1 hour, the solvent is evaporated off under reduced pressure and the solid is taken up in 200 ml of dichloromethane. The solution is subsequently washed with 100 ml of water and then with 100 ml of a saturated sodium chloride solution. After customary treatment of the organic phase, an oil is obtained which is taken up in 500 ml of diethyl ether, and the whole is left in a refrigerator for 2 days. After filtration, the expected product is obtained.

後処理

  1. customthe solvent is evaporated off under reduced pressure
  2. washThe solution is subsequently washed with 100 ml of water
  3. customAfter customary treatment of the organic phase, an oil is obtained which
  4. waitthe whole is left in a refrigerator for 2 days
  5. filtrationAfter filtration

出典と根拠

ORDレコード
ord-b176f1137830430bae59f30d7ccaaa13
出典データセット
uspto-grants-1999_03
特許番号
US05877190

関連ノート

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