Sodium Hydroxide → HCID 12094927, 화합물

HRID 1373988노트

반응식

HRID 1373988 반응식
[C:1]1([C:6]2[CH:7]=[C:8]([CH:14]=[CH:15][CH:16]=2)[C:9](OCC)=[O:10])[CH2:5][CH2:4][CH2:3][CH:2]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3].[OH-].[Na+]>CCOCC>[C:1]1([C:6]2[CH:7]=[C:8]([CH2:9][OH:10])[CH:14]=[CH:15][CH:16]=2)[CH2:5][CH2:4][CH2:3][CH:2]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 12094926Ethyl 3-cyclopenten-1-ylbenzoateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 12094927HCID 12094927, 화합물수율 64.6%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A solution of ethyl 3-cyclopent-1-ylbenzoate (4a) (2.5 g, 12 mmol) in ether (25 ml) is added dropwise to a suspension at 0° C. of LiAlH4 (0.57 g, 15 mmol) in ethyl ether (30 ml). The mixture is stirred overnight at room temperature. The reaction mixture is cooled to 0° C. and then 4.1 ml of a 10% aqueous sodium hydroxide solution are added dropwise. The white precipitate formed is filtered under vacuum, the solid washed with ether and then the filtrate concentrated under reduced pressure. The residue is purified by flash chromatography on silica gel (cyclohexane/ethyl acetate: 90/10). The title product (1.35 g) is obtained in the form of a colorless oil.

후처리

  1. temperatureThe reaction mixture is cooled to 0° C.
  2. customThe white precipitate formed
  3. filtrationis filtered under vacuum
  4. washthe solid washed with ether
  5. concentrationthe filtrate concentrated under reduced pressure
  6. customThe residue is purified by flash chromatography on silica gel (cyclohexane/ethyl acetate: 90/10)

출처 및 근거

ORD 기록
ord-e6623e3e22bf4f1d95bd37f4cc704c0a
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07163957B2

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