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

HRID 372254

반응식

HRID 372254 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 124029792-Chloro-5-methylbenzene-1,3-diamine수율 70%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-d0d14ab86adc40c286ba14ab36a0453d
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04089973

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