Sulfuric Acid → 1-Azido-5-chloro-2,4-dimethoxybenzene

HRID 12438노트

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HRID 12438 반응식
OS(O)(=O)=O.[Cl:6][C:7]1[C:8]([O:16][CH3:17])=[CH:9][C:10]([O:14][CH3:15])=[C:11]([NH2:13])[CH:12]=1.N([O-])=O.[Na+].[N-:22]=[N+:23]=[N-].[Na+]>O>[N:13]([C:11]1[CH:12]=[C:7]([Cl:6])[C:8]([O:16][CH3:17])=[CH:9][C:10]=1[O:14][CH3:15])=[N+:22]=[N-:23]

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 33557Sodium AzideHCID 668075-Chloro-2,4-dimethoxyanilineHCID 23668193Sodium Nitrite

생성물 1

HCID 587310171-Azido-5-chloro-2,4-dimethoxybenzene

시약·촉매·용매 1

HCID 962Water용매4회

반응 조건

온도
0 °C

실험 절차

To a solution of concentrated H2SO4 (5 mL) in water (15 mL), 5-chloro-2,4-dimethoxy-phenylamine (3 g, 16 mmol) was added, resulting a deep purple suspension. More water (15 mL) was then added and the mixture was cooled and stirred vigorously at 0° C. in an ice-salt bath. A solution of sodium nitrite (1.2 g, 17.4 mmol) in water (5 mL) was added slowly and a brown solution was obtained. This solution was stirred at this temperature for an hour. After that, a solution of sodium azide (1.2 g, 18.5 mmol) in water (10 mL) was followed and the solution turned grey. This solution was then stirred for an hour. The grey precipitations (1.0 g, 30%) formed were collected, washed with water and dried. Yellow solids formed in the filtrate were also collected, washed and dried. The second crop (1.47 g, 43%) turned to light grey quickly.

후처리

  1. customresulting a deep purple suspension
  2. temperaturethe mixture was cooled
  3. customa brown solution was obtained
  4. stirringThis solution was stirred at this temperature for an hour
  5. stirringThis solution was then stirred for an hour
  6. customThe grey precipitations (1.0 g, 30%)
  7. customformed
  8. customwere collected
  9. washwashed with water
  10. customdried
  11. customYellow solids formed in the filtrate
  12. customwere also collected
  13. washwashed
  14. customdried

출처 및 근거

ORD 기록
ord-71fdf134242643dab57ea5ca4a673cc1
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728016B2

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