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Malonate Ion → 2-(2-Bromoallyl)propane-1,3-diol

HRID 73428
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HRID 73428 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Br:7][C:8](=[CH2:19])[CH2:9][CH:10]([C:15](OC)=[O:16])[C:11](OC)=[O:12].C([O-])(=O)CC([O-])=O>C(OCC)C>[Br:7][C:8](=[CH2:19])[CH2:9][CH:10]([CH2:15][OH:16])[CH2:11][OH:12]
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참가 물질

5

반응물 3

HCID 9084Malonate IonHCID 11054093Dimethyl 2-(2-bromoallyl)malonateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 593863522-(2-Bromoallyl)propane-1,3-diol수율 86%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

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온도
-78 °C

실험 절차

Lithium aluminum hydride (1.9 g, 7.65 mmol) was slurried in anhydrous diethyl ether (50 ml) and cooled to −78° C. in a dry ice/acetone bath. A solution of the product from step A (0.639 g, 16.84 mmol) in dry ether (26 ml) was then added dropwise. After the malonate was added, the solution was allowed warm to room temperature and stirring was continued for 3 hours. The reaction was quenched with brine (50 ml), extracted with ethyl acetate (3×25 ml) and dried over MgSO4. The solvent was removed in vacuo to give the desired product (1.3 g, 86%) which was used for the next step without further purification. 1H-NMR (300 MHz, CDCl3) δ 5.66 (d, J=1.2 Hz, 1H), 5.48 (d, J=1.5 Hz, 1H), 3.86 (m, 2H), 3.73 (m, 2H), 2.51 (d, J=7.5 Hz, 2H), 2.40 (br s, 2H), 2.15 (m, 1H).

후처리

  1. temperaturethe solution was allowed warm to room temperature
  2. customThe reaction was quenched with brine (50 ml)
  3. extractionextracted with ethyl acetate (3×25 ml)
  4. dry with materialdried over MgSO4
  5. customThe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-29302142d3da4d53a33eb3470f82bc42
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08829052B2

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