2-Pyridinemethanamine → Methyl 4-(2-(2-picolylamino)ethyl)benzoate

HRID 11841

反応式

HRID 11841 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][NH2:8].C(N(C(C)C)CC)(C)C.Br[CH2:19][CH2:20][C:21]1[CH:30]=[CH:29][C:24]([C:25]([O:27][CH3:28])=[O:26])=[CH:23][CH:22]=1>C1(C)C=CC=CC=1>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][NH:8][CH2:19][CH2:20][C:21]1[CH:30]=[CH:29][C:24]([C:25]([O:27][CH3:28])=[O:26])=[CH:23][CH:22]=1

参加物

5

反応物 3

HCID 195092-PyridinemethanamineHCID 81531DiisopropylethylamineHCID 10586287Methyl 4-(2-bromoethyl)benzoate

生成物 1

HCID 21973687Methyl 4-(2-(2-picolylamino)ethyl)benzoate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
80 °C

実験手順

Commercially available 2-picolylamine (0.625 ml) was dissolved in toluene (15 ml) and diisopropylethylamine (0.715 ml) was added. After the addition of the compound obtained in Example 9-1 (499.7 mg), the mixture was stirred for two days at 80° C. After the reaction, toluene was added. The solution was washed with distilled water and saturated brine, and dried over anhydrous sodium sulfate. The solvent was removed by istillation under reduced pressure, and the residue was purified by silica gel column chromatography (25 g, chloroform/methanol=25/1) to obtain the title compound (400.1 mg) as light brown oil.

後処理

  1. additionwas added
  2. washThe solution was washed with distilled water and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was removed by istillation under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (25 g, chloroform/methanol=25/1)

出典と根拠

ORDレコード
ord-a78758e5b0fc4b538301b9f611812224
出典データセット
uspto-grants-2006_08
特許番号
US07098215B2

関連ノート

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