Nitric Acid → 5-Nitro-1,10-phenanthroline

HRID 1180682

반응식

HRID 1180682 반응식
S(=O)(=O)(O)O.[N:6]1[C:19]2[C:10](=[CH:11][CH:12]=[C:13]3[C:18]=2[N:17]=[CH:16][CH:15]=[CH:14]3)[CH:9]=[CH:8][CH:7]=1.[N+:20]([O-])([OH:22])=[O:21].[OH-].[Na+]>O>[N+:20]([C:11]1[CH:12]=[C:13]2[C:18]([N:17]=[CH:16][CH:15]=[CH:14]2)=[C:19]2[C:10]=1[CH:9]=[CH:8][CH:7]=[N:6]2)([O-:22])=[O:21]

참가 물질

6

반응물 4

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 13181,10-PhenanthrolineHCID 14798Sodium Hydroxide

생성물 1

HCID 727905-Nitro-1,10-phenanthroline수율 68%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

Referring to Scheme 5, 237 ml sulfuric acid (concentrate) was first added to a 1 L three-necked flask. 35 g 1,10-phenanthroline was then added into the flask, and the temperature of mixture was kept lower than 100° C. Next, 2436 ml (67%) HNO3 was added drop by drop, and the temperature of mixture was kept lower than 110° C. The mixture was subsequently heated to 100° C. and stirred overnight. After completion of reaction, the reaction mixture was cooled to room temperature and placed into 2 L water, and then NaOH(aq) was added to adjust pH value to a range from 6 to 7, so as to give solids. The solids were washed by water, and dried to obtain solids 5-nitro-1,10-phenanthroline 30 g (0.13 mol, yield 68%).

후처리

  1. additionwas first added to a 1 L three-necked flask
  2. customwas kept lower than 100° C
  3. customwas kept lower than 110° C
  4. customAfter completion of reaction
  5. temperaturethe reaction mixture was cooled to room temperature
  6. customso as to give solids
  7. washThe solids were washed by water
  8. customdried

출처 및 근거

ORD 기록
ord-7ec48b0793ae48f98104c4ecd89ad208
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07282586B1

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