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Ethyl 3-(dimethylamino)-2-(4-hexylphenyl)acrylate → HCID 178442351、化合物

HRID 244952
ノート
印刷プレビュー

反応式

HRID 244952 の反応式
CN(C)C=[C:4]([C:10]1[CH:15]=[CH:14][C:13]([CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])=[CH:12][CH:11]=1)[C:5](OCC)=[O:6].[CH3:23][C:24]([NH:34][NH:35][C:36](OC(C)(C)C)=O)([CH3:33])[CH2:25][C:26]1[CH:31]=[CH:30][C:29]([CH3:32])=[CH:28][CH:27]=1>C(O)(=O)C.C(OCC)C>[CH2:16]([C:13]1[CH:12]=[CH:11][C:10]([C:4]2[CH:36]=[N:35][N:34]([C:24]([CH3:23])([CH3:33])[CH2:25][C:26]3[CH:27]=[CH:28][C:29]([CH3:32])=[CH:30][CH:31]=3)[C:5]=2[OH:6])=[CH:15][CH:14]=1)[CH2:17][CH2:18][CH2:19][CH2:20][CH3:21]
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

5

反応物 2

HCID 86697470Ethyl 3-(dimethylamino)-2-(4-hexylphenyl)acrylateHCID 86697472Tert-butyl 2-(2-methyl-1-(p-tolyl)propan-2-yl)hydrazinecarboxylate

生成物 1

HCID 178442351HCID 178442351、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒2 回HCID 3283Diethyl Ether溶媒

反応条件

温度
90 °C

実験手順

Ethyl 3-(dimethylamino)-2-(4-hexylphenyl)acrylate and 0.50 g (1.8 mmol) of tert-butyl 2-(2-methyl-1-(p-tolyl)propan-2-yl)hydrazinecarboxylate were dissolved in 2 mL of acetic acid and stirred at 90° C. for 24 hours. After the stirring, the reaction mixture was mixed with 0.5 mL of acetic acid and stirred for 48 hours. After completion of the reaction, the reaction mixture was cooled to room temperature, diluted with diethyl ether and washed with distilled water, with saturated aqueous sodium hydrogen carbonate and with saturated aqueous sodium chloride successively. The organic layer was dried over anhydrous sodium sulfate and filtered, and the filtrate was concentrated under reduced pressure. The resulting residue was purified by intermediate pressure silica gel column chromatography (silica gel 30 g, ethyl acetate:hexane=0:100 to 35:65). The resulting solid was washed with isopropyl ether to give 164 mg of the desired product as a white solid.

後処理

  1. stirringstirred for 48 hours
  2. customAfter completion of the reaction
  3. temperaturethe reaction mixture was cooled to room temperature
  4. washwashed with distilled water, with saturated aqueous sodium hydrogen carbonate and with saturated aqueous sodium chloride successively
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationthe filtrate was concentrated under reduced pressure
  8. customThe resulting residue was purified by intermediate pressure silica gel column chromatography (silica gel 30 g, ethyl acetate:hexane=0:100 to 35:65)
  9. washThe resulting solid was washed with isopropyl ether

出典と根拠

ORDレコード
ord-7894eb2ebe044972a9dd513290bbc7e4
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08658686B2

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