Lithium Hydroxide → HCID 10220726、化合物

HRID 2119429ノート

反応式

HRID 2119429 の反応式
[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]

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 15839201HCID 15839201、化合物

生成物 1

HCID 10220726HCID 10220726、化合物収率 50.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
40 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-8b9ebabd5ab847fc8539eed29b7d4468
出典データセット
uspto-grants-2004_02
特許番号
US06686369B1

反応ノート

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