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Ammonia → HCID 20520021, 화합물

HRID 1076270
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HRID 1076270 반응식
C([CH:3]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:4]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[C:6]([Cl:13])[N:5]=1)#N.[O-:20]C#N.[K+].OO.[Mn]([O-])(=O)(=O)=O.N>CC(C)=O.O>[C:3]([C:4]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[C:6]([Cl:13])[N:5]=1)(=[O:20])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 222AmmoniaHCID 784Hydrogen PeroxideHCID 24401PermanganateHCID 11378442Potassium cyanateHCID 20520018HCID 20520018, 화합물

생성물 1

HCID 20520021HCID 20520021, 화합물

시약·촉매·용매 2

HCID 180
Acetone
용매
HCID 962Water용매2회

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온도
15 °C

실험 절차

Five hundred forty eight grams (2 moles) of 2-(cyanophenylmethyl)-3-nitro-6-chloropyridine were suspended in 3 liters of acetone and these were simultaneously dropped in at 37°C. a solution of 325 grams of potassium cyanate (4 moles) in 1 liter of water and a solution of 435 ml of 30% H2O2 (4.05 moles) in 800 ml of water. The reaction vessel was cooled with ice water. Both solutions were added within 45 minutes. After the end of the addition the color of the solution turned from the initial permanganate color (violet) solution to a light yellow. The solution was cooled in an ice bath to 15°C., then 600 grams of ice, 300 ml of 25% aqueous ammonia and 1 liter added with stirring. Yellow crystals separated out. They were filtered off with suction after 1 hour and washed with water. After boiling with 4 parts of methanol per part of crystals, cooling and filtering with suction there was obtained the pure 2-benzoyl-3-nitro-6-chloropyridine, M.P. 107°C.

후처리

  1. additionBoth solutions were added within 45 minutes
  2. additionAfter the end of the addition the color of the solution
  3. customYellow crystals separated out
  4. filtrationThey were filtered off with suction after 1 hour
  5. washwashed with water
  6. temperaturecooling
  7. filtrationfiltering with suction

출처 및 근거

ORD 기록
ord-7e60f04058e141638f36850b95b0697a
출처 데이터셋
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03956344

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