Nitric Acid → HCID 22019211, 화합물

HRID 1442894노트

반응식

HRID 1442894 반응식
[N+:1]([O-:4])(O)=[O:2].[CH3:5][C:6]1[CH:7]=[N:8][CH:9]=[CH:10][C:11]=1[O:12][CH3:13].C(=O)([O-])[O-].[K+].[K+]>S(=O)(=O)(O)O>[CH3:5][C:6]1[CH:7]=[N:8][CH:9]=[C:10]([N+:1]([O-:4])=[O:2])[C:11]=1[O:12][CH3:13]

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 11430Potassium Carbonate2회HCID 47377664-Methoxy-3-methylpyridine

생성물 1

HCID 22019211HCID 22019211, 화합물수율 30%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

30 ml of 100% nitric acid is added to 150 ml of 98% sulphuric acid with stirring and cooling. To this solution is added dropwise 3.2 g (26 mmol) of 3-methyl-4-methoxy pyridine. The mixture is stirred at 80° C. for 2.5 hours, cooled down and added cautiously to a mixture of 400 g of crushed ice and 300 g of potassium carbonate with external cooling. 125 g more of potassium carbonate is added, and the suspension is filtered. The cake is washed with around 11 of diethyl ether. The filtrate layers are separated, the ethereal layer is dried, filtered off and concentrated to give 2.9 g (30% yield) of a yellow oil (M+1=169) (purity #80%, used with no further purification).

후처리

  1. temperaturecooling
  2. stirringThe mixture is stirred at 80° C. for 2.5 hours
  3. temperaturecooled down
  4. filtrationthe suspension is filtered
  5. washThe cake is washed with around 11 of diethyl ether
  6. customThe filtrate layers are separated
  7. customthe ethereal layer is dried
  8. filtrationfiltered off
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-0d80e3031c37456699b12033f46d0ee1
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07659307B2

반응 노트

불러오는 중…