过氧化钠 → 2-[(E)-tert-Butyldiazenyl]-4-methylpentane-2-peroxol

HRID 596140

反应方程式

HRID 596140 反应方程式
[O-:1][O-:2].[Na+].[Na+].[C:5]([N:9]=[N:10][C:11](Cl)([CH2:13][CH:14]([CH3:16])[CH3:15])[CH3:12])([CH3:8])([CH3:7])[CH3:6]>CO>[C:5]([N:9]=[N:10][C:11]([O:1][OH:2])([CH2:13][CH:14]([CH3:16])[CH3:15])[CH3:12])([CH3:8])([CH3:7])[CH3:6]

参与物

4

反应物 2

HCID 14803过氧化钠HCID 23344796(E)-1-tert-Butyl-2-(2-chloro-4-methylpentan-2-yl)diazene

产物 1

HCID 234664402-[(E)-tert-Butyldiazenyl]-4-methylpentane-2-peroxol

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 stirred solution of 1.56g (.02 moles) of sodium peroxide in 30 ml. of 75% aqueous methanol in a 50 ml. erlenmeyer flask immersed in a cold water bath, was added 4.1g (.02 moles) of 2-t-butylazo-2-chloro-4-methylpentane dropwise. After the addition was complete, the reaction mixture was stirred for an additional 45 minutes and poured into ice water containing 0.02 moles of HaSO4. The product was extracted with pentane and washed with cold solutions of ammonium sulfate and sodium bicarbonate, washed with water, dried over anhydrous sodium sulfate, filtered and the pentane stripped off under reduced pressure while the flask was immersed in an ice bath. The yield was 2.7 grams (67% of theory) and the product began to decompose when allowed to warm to room temperature. The infrared spectrum showed the characteristic hydroperoxide absorption at 3300-3400 cm-1.

后处理

  1. customerlenmeyer flask immersed in a cold water bath
  2. additionAfter the addition
  3. extractionThe product was extracted with pentane
  4. washwashed with cold solutions of ammonium sulfate and sodium bicarbonate
  5. washwashed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. customwas immersed in an ice bath
  9. customthe characteristic hydroperoxide absorption at 3300-3400 cm-1

来源与证据

ORD记录
ord-0810142252724805b7fbb3e08136a5d9
来源数据集
uspto-grants-1977_03
专利号
US04010152

关联笔记

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