3-Nitroaniline → Benzamide, 3-nitro-N-(3-nitrophenyl)-

HRID 263051

反応式

HRID 263051 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:8]=[CH:9][CH:10]=1)[NH2:7])([O-:3])=[O:2].C(N(CC)CC)C.[N+:18]([C:21]1[CH:22]=[C:23]([CH:27]=[CH:28][CH:29]=1)[C:24](Cl)=[O:25])([O-:20])=[O:19]>C(OCC)(=O)C>[N+:18]([C:21]1[CH:22]=[C:23]([CH:27]=[CH:28][CH:29]=1)[C:24]([NH:7][C:6]1[CH:8]=[CH:9][CH:10]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=1)=[O:25])([O-:20])=[O:19]

参加物

5

反応物 3

HCID 74233-NitroanilineHCID 8471TriethylamineHCID 8495Benzoyl chloride, 3-nitro-

生成物 1

HCID 66861Benzamide, 3-nitro-N-(3-nitrophenyl)-

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

To a stirred solution of 13.81 g. (0.1 mole) of m-nitroaniline in 100 ml. of dry ethyl acetate is added 11.13 g. (0.11 mole) of triethylamine. To the solution is added a solution of 18.56 g. (0.1 mole) of m-nitrobenzoylchloride in 100 ml of ethyl acetate. The mixture is refluxed for 6.5 hours. The reaction mixture is allowed to stand at room temperature overnight. The precipitate is removed by filtration. The filtrate is evaporated to dryness in vacuo. The residue is recrystallized from absolute ethanol. There is obtained 5.79 g. of yellow needles that melt at 188°-189°.

後処理

  1. additionTo the solution is added a solution of 18.56 g
  2. temperatureThe mixture is refluxed for 6.5 hours
  3. customThe precipitate is removed by filtration
  4. customThe filtrate is evaporated to dryness in vacuo
  5. customThe residue is recrystallized from absolute ethanol
  6. customThere is obtained 5.79 g
  7. customthat melt at 188°-189°

出典と根拠

ORDレコード
ord-09b7fed3dbea424fbb90fc3a8fea118c
出典データセット
uspto-grants-1979_05
特許番号
US04156012

関連ノート

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