Sodium peroxide → HCID 20367916, 화합물

HRID 616580

반응식

HRID 616580 반응식
[O-:1][O-:2].[Na+].[Na+].[C:5]([N:9]=[N:10][C:11]1(Cl)[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1)([CH3:8])([CH3:7])[CH3:6]>CO>[C:5]([N:9]=[N:10][C:11]1([O:1][O:2][C:11]2([N:10]=[N:9][C:5]([CH3:8])([CH3:7])[CH3:6])[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]2)[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1)([CH3:8])([CH3:7])[CH3:6]

참가 물질

4

반응물 2

HCID 14803Sodium peroxideHCID 233447841-t-Butylazo-1-chlorocyclohexane

생성물 1

HCID 20367916HCID 20367916, 화합물수율 100.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 0.78 grams (.01 moles) of sodium peroxide in 30 ml. of methanol, cooled to 10° C in a 50 ml. erlenmeyer flask immersed in a cold water bath was added 4.3 grams (.0213 moles) of 1-t-butylazo-1-chlorocyclo-hexane dropwise and with rapid stirring holding the temperature at 10°-15° C. After the addition was complete, the reaction was stirred for 1 hour at 5° C. It was then poured in 250 ml. of ice cold water and the product extracted with pentane. The pentane layer was separated, washed with saturated (NH4)2SO4, water, saturated NaHCO3, water, dried, filtered and the pentane evaporated under reduced pressure to give 3.67 grams (85% yield) of crude di[1-(t-butylazo)cyclohexyl] peroxide. The infrared spectrum indicated the product was contaminated to a small extent by 1-t-butylazo-1-methoxy-cyclohexane which resulted from the chloro compound reacting to a small extent with the methanol solvent.

후처리

  1. customerlenmeyer flask immersed in a cold water bath
  2. customat 10°-15° C
  3. additionAfter the addition
  4. stirringthe reaction was stirred for 1 hour at 5° C
  5. additionIt was then poured in 250 ml
  6. extractionof ice cold water and the product extracted with pentane
  7. customThe pentane layer was separated
  8. washwashed with saturated (NH4)2SO4, water, saturated NaHCO3, water
  9. customdried
  10. filtrationfiltered
  11. customthe pentane evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-4648701b3c0c48e7a5cd47961c5580c5
출처 데이터셋
uspto-grants-1978_02
특허 번호
US04075199

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