Acetic Acid → HCID 86657893、化合物

HRID 1045345

反応式

HRID 1045345 の反応式
[N+:1]([CH2:4][C:5]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)=O)([O-:3])=[O:2].O.[NH2:14][NH2:15].C(O)(=O)C>C(O)C>[N+:1]([CH2:4][C:5](=[N:14][NH2:15])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)([O-:3])=[O:2]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 24654Hydrazine hydrate (1:1)HCID 948332-Nitro-1-phenylethanone

生成物 1

HCID 86657893HCID 86657893、化合物収率 81.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 2-nitroacetophenone (12.28 g, 0.074 mol) in ethanol (100 mL) was treated with hydrazine hydrate (10.24 g, 0.163 mol) and glacial acetic acid (4.2 mL, 0.074 mol) and the mixture was heated at reflux for 3 hours. The solvent was then evaporated in vacuo. The residue was dissolved in trichloromethane and extracted three times with water to remove the excess of hydrazine hydrate. Evaporation of the organic layer yielded the product (11 g, 0.06 mol, 81%), which was used in the next step without further purification.

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 3 hours
  3. customThe solvent was then evaporated in vacuo
  4. dissolutionThe residue was dissolved in trichloromethane
  5. extractionextracted three times with water
  6. customto remove the excess of hydrazine hydrate
  7. customEvaporation of the organic layer

出典と根拠

ORDレコード
ord-f717f6b035134c5f95e546611fba502b
出典データセット
uspto-grants-2013_10
特許番号
US08569259B2

関連ノート

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