Sodium Succinate → HCID 53682371, 화합물

HRID 1578576

반응식

HRID 1578576 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 53682371HCID 53682371, 화합물수율 60%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a51a7cee7c564a30aeec9185cee663d7
출처 데이터셋
uspto-grants-1976_02
특허 번호
US03937761

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