Hydrochloric Acid → 5-Nitro-2-(1-pyrrolidinyl)benzenamine

HRID 349734ノート

反応式

HRID 349734 の反応式
[N+:1]([C:4]1[CH:5]=[CH:6][C:7]([N:14]2[CH2:18][CH2:17][CH2:16][CH2:15]2)=[C:8]([NH:10]C(=O)C)[CH:9]=1)([O-:3])=[O:2].Cl.[OH-].[Na+]>C(OCC)(=O)C>[N+:1]([C:4]1[CH:5]=[CH:6][C:7]([N:14]2[CH2:18][CH2:17][CH2:16][CH2:15]2)=[C:8]([CH:9]=1)[NH2:10])([O-:3])=[O:2]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 609964HCID 609964、化合物

生成物 1

HCID 129083915-Nitro-2-(1-pyrrolidinyl)benzenamine

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

0.58 g (2.3 mmol) of N-(5-nitro-2-pyrrolidin-1-ylphenyl)acetamide was admixed with 12 ml of conc. hydrochloric acid and heated to reflux for 1.5 hours. The solution was added to 100 ml of ice/water, neutralized with 2 N sodium hydroxide solution and admixed three times with ethyl acetate. After the mixture had been dried, the solvent was distilled off under reduced pressure to obtain the product quantitatively as a red solid which was used for the reactions a-d described in Example 1 without further purification (reaction with the acyl isocyanate, reduction with SnCl2 and acylation with Ac2O).

後処理

  1. temperatureheated
  2. temperatureto reflux for 1.5 hours
  3. customAfter the mixture had been dried
  4. distillationthe solvent was distilled off under reduced pressure
  5. customto obtain the product quantitatively as a red solid which
  6. customdescribed in Example 1 without further purification (
  7. customreaction with the acyl isocyanate, reduction with SnCl2 and acylation with Ac2O)

出典と根拠

ORDレコード
ord-c211579ec17544f3acd4387814493215
出典データセット
uspto-grants-2007_02
特許番号
US07179941B2

反応ノート

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