Potassium Bromide → (S)-2-bromo-4-methylpentanoic acid

HRID 264978

반응식

HRID 264978 반응식
[Br-:1].[K+].N[C@@H:4]([C:9]([OH:11])=[O:10])[CH2:5][CH:6]([CH3:8])[CH3:7].N([O-])=O.[Na+]>S(=O)(=O)(O)O>[Br:1][C@@H:4]([CH2:5][CH:6]([CH3:8])[CH3:7])[C:9]([OH:11])=[O:10]

참가 물질

5

반응 조건

온도
-10 °C

실험 절차

Potassium bromide (9.5 g., 80 mmol.) was added to a stirred solution of D-leucine (3.0 g., 23 mmol.) in 2.5N sulfuric acid (47 ml.) at room temperature. The reaction mixture was cooled to -10° C. and solid sodium nitrite (2.4 g., 34 mmol.) was added portionwise, maintaining the temperature between -10° and -5° C. After addition was complete, the reaction was stirred for 1 hour and then warmed to room temperature and stirred for another hour. The reaction mixture was then extracted twice with ether, the ether extracts were washed once with water, dried (magnesium sulfate), filtered and evaporated to give 2.7 g. of crude title product.

후처리

  1. temperaturemaintaining the temperature between -10° and -5° C
  2. additionAfter addition
  3. temperaturewarmed to room temperature
  4. stirringstirred for another hour
  5. extractionThe reaction mixture was then extracted twice with ether
  6. washthe ether extracts were washed once with water
  7. dry with materialdried (magnesium sulfate)
  8. filtrationfiltered
  9. customevaporated
  10. customto give 2.7 g

출처 및 근거

ORD 기록
ord-f61706e6f3f34088a315daa06993d596
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05646276

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