Sodium Succinate → Di(1-t-butylazo-1,3-dimethylbutyl) Succinate

HRID 1578576ノート

反応式

HRID 1578576 の反応式
[C:1]([O-:8])(=[O:7])[CH2:2][CH2:3][C:4]([O-:6])=[O:5].[Na+].[Na+].[C:11]([N:15]=[N:16][C:17](Cl)([CH2:19][CH:20]([CH3:22])[CH3:21])[CH3:18])([CH3:14])([CH3:13])[CH3:12]>CN(C)C=O>[C:1]([O:8][C:17]([N:16]=[N:15][C:11]([CH3:14])([CH3:13])[CH3:12])([CH3:18])[CH2:19][CH:20]([CH3:21])[CH3:22])(=[O:7])[CH2:2][CH2:3][C:4]([O:6][C:17]([N:16]=[N:15][C:11]([CH3:14])([CH3:13])[CH3:12])([CH3:18])[CH2:19][CH:20]([CH3:22])[CH3:21])=[O:5]

参加物

4

反応物 2

HCID 9020Sodium SuccinateHCID 23344796(E)-1-tert-Butyl-2-(2-chloro-4-methylpentan-2-yl)diazene

生成物 1

HCID 53682371Di(1-t-butylazo-1,3-dimethylbutyl) Succinate収率 60%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a slurry of 5.97 grams (.0221 moles) of sodium succinate in 75 mls. of dimethylformamide in a 200 beaker, warmed to 35°C in a water bath, was added 9.0 grams (.0442 moles) of 2-t-butylazo-2-chloro-4-methylpentane dropwise. After the addition was complete, the reaction was stirred for 3 hours at room temperature, poured into 200 ml. of cold water and extracted with pentane. The pentane solution was washed with water, dried over anhydrous Na2SO4, filtered, stirred over alumina, filtered and the pentane evaporated to leave 6.0 grams (60% yield) of a light yellow liquid. The crude product was purified by column chromatography using pentane as eluent. The infrared spectrum of the purified product was in agreement with the structure of the desired product.

後処理

  1. additionAfter the addition
  2. additionpoured into 200 ml
  3. extractionof cold water and extracted with pentane
  4. washThe pentane solution was washed with water
  5. dry with materialdried over anhydrous Na2SO4
  6. filtrationfiltered
  7. stirringstirred over alumina
  8. filtrationfiltered
  9. customthe pentane evaporated

出典と根拠

ORDレコード
ord-a51a7cee7c564a30aeec9185cee663d7
出典データセット
uspto-grants-1976_02
特許番号
US03937761

反応ノート

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