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

HRID 848503

反応式

HRID 848503 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-88dd2d6a25ba406ead5f84d5b32ec26a
出典データセット
uspto-grants-1981_10
特許番号
US04296120

関連ノート

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