Kojic Acid → Chlorokojic acid

HRID 259841

반응식

HRID 259841 반응식
[CH:1]1[C:6](=[O:7])[C:5]([OH:8])=[CH:4][O:3][C:2]=1[CH2:9]O.S(Cl)([Cl:13])=O>CN(C)C=O>[CH:1]1[C:6](=[O:7])[C:5]([OH:8])=[CH:4][O:3][C:2]=1[CH2:9][Cl:13]

참가 물질

4

반응물 2

HCID 3840Kojic AcidHCID 24386Thionyl Chloride

생성물 1

HCID 82051Chlorokojic acid수율 66.83%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
10 °C

실험 절차

50 g(351.8 mmol) of kojic acid was dissolved in 250 ml of N,N-dimethylformamide. The resulting solution was cooled in a ice bath of 10° C. and 30 ml(411.3 mmole) of thionyl chloride was added dropwise thereto. The mixture was stirred at a room temperature for 2 hours and 2000 ml of ice water was added. The precipitates were filtered and dissolved into 1000 ml of ethyl acetate. The reaction product was dried over magnesium sulfate, decolored with active charcoal and filtered. The filtrate was concentrated and hexane was added to give crystals, which was then dried under vacuum to give 37.5 g(66.83%) of the desired chlorokojic acid as a yellow solid.

후처리

  1. filtrationThe precipitates were filtered
  2. dissolutiondissolved into 1000 ml of ethyl acetate
  3. dry with materialThe reaction product was dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated
  6. additionhexane was added
  7. customto give crystals, which
  8. customwas then dried under vacuum

출처 및 근거

ORD 기록
ord-8e4894ec7a404f27b9bad3889dbbf050
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05523421

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