Lithium Hydroxide → HCID 10220726, 화합물

HRID 2119429노트

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HRID 2119429 반응식
[OH:1][CH:2]([C:8]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[CH3:9])[C:3]([O:5]CC)=[O:4].[Li+].[OH-]>C1COCC1.O>[OH:1][CH:2]([C:8]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)([C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1)[CH3:9])[C:3]([OH:5])=[O:4]

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 15839201HCID 15839201, 화합물

생성물 1

HCID 10220726HCID 10220726, 화합물수율 50.3%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
40 °C

실험 절차

1.75 g (6.2 mmol) of ethyl 2-hydroxy-3,3-diphenylbutyrate were dissolved in 10 ml of THF, and a solution of 0.23 g (9.3 mmol) of LiOH in 6 ml of water was added. The mixture was stirred at room temperature for 16 hours and at 40° C. for 4 hours. The mixture was subsequently concentrated under reduced pressure, taken up in water and washed with ethyl acetate. This was followed by acidification with HCl and extraction three times with ethyl acetate. The combined ethyl acetate phases were dried with MgSO4, and the solvent was stripped off under reduced pressure. The residue was chromatographed on silica gel with CH2Cl2/MeOH (2:1). 0.80 g (50%) of 2-hydroxy-3,3-diphenylbutyric acid was obtained.

후처리

  1. concentrationThe mixture was subsequently concentrated under reduced pressure
  2. washwashed with ethyl acetate
  3. extractionThis was followed by acidification with HCl and extraction three times with ethyl acetate
  4. dry with materialThe combined ethyl acetate phases were dried with MgSO4
  5. customThe residue was chromatographed on silica gel with CH2Cl2/MeOH (2:1)

출처 및 근거

ORD 기록
ord-8b9ebabd5ab847fc8539eed29b7d4468
출처 데이터셋
uspto-grants-2004_02
특허 번호
US06686369B1

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