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Dimethylformamide dimethyl acetal → Ethyl 3-(dimethylamino)-2-(4-hexylphenyl)acrylate

HRID 1504290
ノート
印刷プレビュー

反応式

HRID 1504290 の反応式
[CH2:1]([C:7]1[CH:12]=[CH:11][C:10]([CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:9][CH:8]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].CO[CH:21](OC)[N:22]([CH3:24])[CH3:23]>CN(C)C=O.C(OCC)C>[CH3:21][N:22]([CH3:24])[CH:23]=[C:13]([C:10]1[CH:11]=[CH:12][C:7]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6])=[CH:8][CH:9]=1)[C:14]([O:16][CH2:17][CH3:18])=[O:15]
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 78373Dimethylformamide dimethyl acetal2 回HCID 3703215Ethyl 2-(4-hexylphenyl)acetate

生成物 1

HCID 86697470Ethyl 3-(dimethylamino)-2-(4-hexylphenyl)acrylate

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

0.50 g (2.0 mmol) of ethyl 2-(4-hexylphenyl)acetate was dissolved in 7 mL of N,N-dimethylformamide, mixed with 0.31 mL (2.3 mmol) of N,N-dimethylformamide dimethyl acetal and stirred at 60° C. for 18 hours. After the stirring, the reaction mixture was further mixed with 0.65 mL (4.9 mmol) of N,N-dimethylformamide dimethyl acetal and stirred at 60° C. for 24 hours. After completion of the reaction, the reaction mixture was diluted with diethyl ether and washed 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 to give the desired product as a brown liquid.

後処理

  1. stirringstirred at 60° C. for 24 hours
  2. customAfter completion of the reaction
  3. washwashed with saturated aqueous sodium hydrogen carbonate and with saturated aqueous sodium chloride successively
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-41c1389c35dd4300b7041d3c3ea7ff51
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09212348B2

反応ノート

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