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(2-Methoxyethyl)(methyl)amine → [4-(2-Bromophenyl)-5-(6-phenylpyridin-3-yl)-4H-1,2,4-triazol-3-yl]-N-(2-methoxyethyl)-N-methylamine

HRID 1797117
ノート
印刷プレビュー

反応式

HRID 1797117 の反応式
[CH3:1][O:2][CH2:3][CH2:4][NH:5][CH3:6].Br[C:8]1[N:9]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=2[Br:31])[C:10]([C:13]2[CH:14]=[CH:15][C:16]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[N:17][CH:18]=2)=[N:11][N:12]=1>C(Cl)(Cl)Cl>[Br:31][C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=1[N:9]1[C:10]([C:13]2[CH:18]=[N:17][C:16]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[CH:15][CH:14]=2)=[N:11][N:12]=[C:8]1[N:5]([CH2:4][CH2:3][O:2][CH3:1])[CH3:6]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 300977(2-Methoxyethyl)(methyl)amineHCID 220192295-[5-bromo-4-(2-bromophenyl)-4H-1,2,4-triazol-3-yl]-2-phenylpyridine

生成物 1

HCID 22019250[4-(2-Bromophenyl)-5-(6-phenylpyridin-3-yl)-4H-1,2,4-triazol-3-yl]-N-(2-methoxyethyl)-N-methylamine収率 70%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
200 °C

実験手順

In a sealed tube, N-(2-methoxyethyl)methylamine (3 ml) was added to 5-[5-bromo-4-(2-bromophenyl)-4H-1,2,4-triazol-3-yl]-2-phenylpyridine (1.0 g) prepared in the Production Example 3, and stirred at 180° C. for 13 hours and at 200° C. for 24 hours. After the reaction solution was cooled to ambient temperature, chloroform was added to the solution, which was then washed with saturated aqueous sodium hydrogen carbonate solution. The organic layer was dried over anhydrous magnesium sulfate. After the solvent was evaporated under reduced pressure, the resulting residue was washed with ethyl acetate, to afford the entitled compound as white solid (711 mg, 70%). The physico-chemical values are as follows.

後処理

  1. customprepared in the Production Example 3
  2. temperatureAfter the reaction solution was cooled to ambient temperature
  3. washwas then washed with saturated aqueous sodium hydrogen carbonate solution
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. customAfter the solvent was evaporated under reduced pressure
  6. washthe resulting residue was washed with ethyl acetate

出典と根拠

ORDレコード
ord-7ae3865481ac4fea8fe65ac34f5a355a
出典データセット
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07034047B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート