(E)-1-tert-Butyl-2-(2-chloro-4-methylpentan-2-yl)diazene → 2-t-Butylazo-2-phenyl-4-methylpentane

HRID 1856392

반응식

HRID 1856392 반응식
[C:1]1([Li])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:8]([N:12]=[N:13][C:14](Cl)([CH2:16][CH:17]([CH3:19])[CH3:18])[CH3:15])([CH3:11])([CH3:10])[CH3:9]>CCOCC>[C:8]([N:12]=[N:13][C:14]([C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)([CH2:16][CH:17]([CH3:19])[CH3:18])[CH3:15])([CH3:11])([CH3:10])[CH3:9]

참가 물질

4

반응물 2

HCID 23344796(E)-1-tert-Butyl-2-(2-chloro-4-methylpentan-2-yl)diazeneHCID 178506676HCID 178506676, 화합물

생성물 1

HCID 233447602-t-Butylazo-2-phenyl-4-methylpentane

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
5 °C

실험 절차

To a clean, dry 250 ml. round bottom 4 neck flask equipped with a magnetic stirrer, thermometer, condenser and addition funnel, which was being purged with nitrogen was added an ether solution containing 0.06 moles of phenyllithium. The solution was cooled to 5° C. and a solution of 10.25 g. (0.05 L moles) of 2-t-butylazo-2-chloro-4-methylpentane in 50 ml. ether was added dropwise over 1/2 hour. After the addition was complete, the reaction was warmed to 20° C. and stirred for 1/2 hour. The excess phenyllithium was destroyed with wet ether and the reaction mixture poured into 200 ml. water. The ether layer was separated, dried over anhydrous sodium sulfate, filtered and the ether removed on a rotating evaporator leaving 11.9 g. (96%) of a liquid. The infrared spectrum was in agreement with the structure of the title compound.

후처리

  1. customTo a clean, dry 250 ml
  2. customround bottom 4 neck flask equipped with a magnetic stirrer
  3. additionthermometer, condenser and addition funnel
  4. customwhich was being purged with nitrogen
  5. additionwas added an ether solution
  6. additionAfter the addition
  7. temperaturethe reaction was warmed to 20° C.
  8. customThe excess phenyllithium was destroyed with wet ether
  9. additionthe reaction mixture poured into 200 ml
  10. customThe ether layer was separated
  11. dry with materialdried over anhydrous sodium sulfate
  12. filtrationfiltered
  13. customthe ether removed on a rotating evaporator
  14. customleaving 11.9 g

출처 및 근거

ORD 기록
ord-5ac7bcae43cd411aa54863baa94cce8d
출처 데이터셋
uspto-grants-1980_08
특허 번호
US04219476

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