Hydrochloric Acid → 2-Chloro-5-methylbenzene-1,3-diamine

HRID 372254

反応式

HRID 372254 の反応式
[Cl:1][C:2]1[C:7]([N+:8]([O-])=O)=[CH:6][C:5]([CH3:11])=[CH:4][C:3]=1[N+:12]([O-])=O.Cl.[OH-].[Na+]>C(O)C>[NH2:12][C:3]1[CH:4]=[C:5]([CH3:11])[CH:6]=[C:7]([NH2:8])[C:2]=1[Cl:1]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 789184-Chloro-3,5-dinitrotoluene

生成物 1

HCID 124029792-Chloro-5-methylbenzene-1,3-diamine収率 70%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

4-chloro-3,5-dinitrotoluene (9.0 gm.) is dissolved in 50% ethanol (30 ml.). Electrolytically reduced iron powder (14.2 gm.) is added and the stirred reaction mixture heated to reflux. Concentrated HCl (1 ml.) in 50 % ethanol (5 ml.) is added dropwise and refluxing continued for one hour. The reaction mixture is allowed to cool slightly and made basic (pH 8) with 20% NaOH, then the iron removed by filtration. The filtrate is taken to dryness under reduced pressure and the residue extracted with hot Skellysolve "B" (700 ml.). The product precipitates in long needles that were collected by filtration (4.57 gm., m.p. 114°-115.5°, 70% yield).

後処理

  1. customthe stirred reaction mixture
  2. temperatureheated to reflux
  3. temperaturerefluxing
  4. temperatureto cool slightly
  5. customthe iron removed by filtration
  6. extractionthe residue extracted with hot Skellysolve "B" (700 ml.)
  7. customThe product precipitates in long needles that
  8. filtrationwere collected by filtration (4.57 gm., m.p. 114°-115.5°, 70% yield)

出典と根拠

ORDレコード
ord-d0d14ab86adc40c286ba14ab36a0453d
出典データセット
uspto-grants-1978_05
特許番号
US04089973

関連ノート

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