Sodium peroxide → 2-[(E)-tert-Butyldiazenyl]-4-methylpentane-2-peroxol

HRID 596140

反応式

HRID 596140 の反応式
[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]

参加物

4

反応物 2

HCID 14803Sodium peroxideHCID 23344796(E)-1-tert-Butyl-2-(2-chloro-4-methylpentan-2-yl)diazene

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0810142252724805b7fbb3e08136a5d9
出典データセット
uspto-grants-1977_03
特許番号
US04010152

関連ノート

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