Octylamine → N-Octyl-3-(2-Nitrophenyl)propenamide

HRID 1065819

반응식

HRID 1065819 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH:10]=[CH:11][C:12]([OH:14])=O)([O-:3])=[O:2].C(N(CC)CC)C.ClC(OCC)=O.[CH2:28]([NH2:36])[CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35]>ClCCl>[CH2:28]([NH:36][C:12](=[O:14])[CH:11]=[CH:10][C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=1[N+:1]([O-:3])=[O:2])[CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35]

참가 물질

6

반응물 4

HCID 8143OctylamineHCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 928203-(2-Nitrophenyl)acrylic acid

생성물 1

HCID 54507938N-Octyl-3-(2-Nitrophenyl)propenamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

A mixture of 9.7 g. of 3-(2-nitrophenyl)propenoic acid, 5.6 g. of triethylamine and 240 ml. of dichloromethane was stirred at room temperature for 20 minutes, and then it was cooled in an ice-bath. To the mixture was then added, dropwise, during 15 minutes, a solution of 6.0 g. of ethyl chloroformate in 20 ml. of dichloromethane. After 15 minutes of stirring, a solution of 7.1 g. of octylamine in 20 ml. of dichloromethane 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 carbonate, 1 N hydrochloric acid, water and saturated sodium chloride. The resulting solution was dried and evaporated in vacuo, leaving 14.5 g. (95%) yield of the title compound as a tan solid.

후처리

  1. additionA mixture of 9.7 g
  2. temperatureit was cooled in an ice-bath
  3. additionTo the mixture was then added
  4. washit was washed successively with 1 N potassium carbonate, 1 N hydrochloric acid, water and saturated sodium chloride
  5. customThe resulting solution was dried
  6. customevaporated in vacuo
  7. customleaving 14.5 g

출처 및 근거

ORD 기록
ord-f9588d446e5f46779e402f6aa1d90871
출처 데이터셋
uspto-grants-1982_05
특허 번호
US04331683

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