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

HRID 66619

반응식

HRID 66619 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 6344Dichloromethane용매3회HCID 8471Triethylamine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-81e276abfb374bdb9227e7392fe57723
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04342781

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