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Decylamine → N-Decyl-3-phenyl-3-(3-nitrophenyl)propenamide

HRID 66619
ノート
印刷プレビュー

反応式

HRID 66619 の反応式
[C:1]1([C:7]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([N+:18]([O-:20])=[O:19])[CH:13]=2)=[CH:8][C:9]([OH:11])=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.ClC(OCC)=O.[CH2:27]([NH2:37])[CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH3:36]>C(Cl)Cl.C(N(CC)CC)C>[CH2:27]([NH:37][C:9](=[O:11])[CH:8]=[C:7]([C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)[C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([N+:18]([O-:20])=[O:19])[CH:13]=1)[CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH3:36]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8916DecylamineHCID 10928Ethyl chloroformateHCID 536864243-Phenyl-3-(3-nitrophenyl)propenoic acid

生成物 1

HCID 53913879N-Decyl-3-phenyl-3-(3-nitrophenyl)propenamide

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒3 回HCID 8471Triethylamine
溶媒

実験手順

To a stirred solution of 8.0 g. of 3-phenyl-3-(3-nitrophenyl)propenoic acid in 260 ml. of methylene chloride was added 3.3 g. of triethylamine. The mixture was stirred for 20 minutes and then it was cooled in an ice-bath. To the cooled solution was added, dropwise, during 15 minutes, a solution of 3.6 g. of ethyl chloroformate in 30 ml. of methylene chloride. Stirring was continued for 20 minutes, and then a solution of 5.2 g. of decylamine in 30 ml. of methylene chloride was added, dropwise, during 10 minutes. The reaction mixture was allowed to warm to room temperature, and then it was washed successively with 1 N potassium hydroxide, 1 N hydrochloric acid, water, and saturated sodium chloride solution. The resulting solution was dried (Na2SO4) and evaporated in vacuo to give the 10.7 g. of the title compound as a oil.

後処理

  1. temperatureit was cooled in an ice-bath
  2. additionTo the cooled solution was added
  3. waitdropwise, during 15 minutes
  4. stirringStirring
  5. waitwas continued for 20 minutes
  6. waitdropwise, during 10 minutes
  7. washit was washed successively with 1 N potassium hydroxide, 1 N hydrochloric acid, water, and saturated sodium chloride solution
  8. dry with materialThe resulting solution was dried (Na2SO4)
  9. customevaporated in vacuo
  10. customto give the 10.7 g

出典と根拠

ORDレコード
ord-81e276abfb374bdb9227e7392fe57723
出典データセット
uspto-grants-1982_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04342781

反応ノート

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