Hydrochloric Acid → N-(5-ethylpyrimidin-4-yl)-4-[3-(1-benzylpiperidin-4-yl)propanoyl]aniline

HRID 976129ノート

反応式

HRID 976129 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][CH2:15][C:16]([C:18]2[CH:24]=[CH:23][C:21]([NH2:22])=[CH:20][CH:19]=2)=[O:17])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[C:26]1[C:31]([CH2:32][CH3:33])=[CH:30][N:29]=[CH:28][N:27]=1.Cl.C[O-].[Na+].CO>C(O)C>[CH2:32]([C:31]1[C:26]([NH:22][C:21]2[CH:20]=[CH:19][C:18]([C:16](=[O:17])[CH2:15][CH2:14][CH:11]3[CH2:12][CH2:13][N:8]([CH2:1][C:2]4[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=4)[CH2:9][CH2:10]3)=[CH:24][CH:23]=2)=[N:27][CH:28]=[N:29][CH:30]=1)[CH3:33]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 199689164-Chloro-5-ethylpyrimidineHCID 199689194-[3-(1-Benzylpiperidin-4-yl)propanoyl]anilineHCID 23694274Sodium methanolate methanol

生成物 1

HCID 19968894N-(5-ethylpyrimidin-4-yl)-4-[3-(1-benzylpiperidin-4-yl)propanoyl]aniline収率 58.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

To 10 ml of ethanol were added 0.23 g of 4-[3-(1-benzylpiperidin-4-yl)propanoyl]aniline and 0.13 g of 4-chloro-5-ethylpyrimidine, and after adding 2 ml of an ethanol solution of hydrochloric acid (containing 0.071 g of hydrochloric acid), the mixture was reacted under reflux for 2 hours. After cooling, a 28% sodium methylate-methanol solution was added to the reaction mixture to make it alkaline, and then the mixture was condensed under reduced pressure. The obtained residue was applied to silica gel column chromatography to obtain 0.18 g of the title compound as pale yellow crystal.

後処理

  1. customthe mixture was reacted
  2. temperatureunder reflux for 2 hours
  3. temperatureAfter cooling
  4. customcondensed under reduced pressure

出典と根拠

ORDレコード
ord-fc8d77730ea844e4a41c0bd46b991193
出典データセット
uspto-grants-1997_03
特許番号
US05610303

反応ノート

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