过氧化钠 → HCID 20367916，化合物

HRID 616580

反应方程式

HRID 616580 反应方程式
[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]

参与物

4

反应物 2

HCID 14803过氧化钠HCID 233447841-t-Butylazo-1-chlorocyclohexane

产物 1

HCID 20367916HCID 20367916，化合物收率 100.1%

试剂、催化剂与溶剂 1

HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-4648701b3c0c48e7a5cd47961c5580c5
来源数据集
uspto-grants-1978_02
专利号
US04075199

关联笔记

加载中…