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Water → HCID 22399035, 화합물

HRID 1647850
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HRID 1647850 반응식
[O:1]=[C:2]([CH3:15])[CH2:3][CH:4]([C:10](OCC)=[O:11])[C:5](OCC)=[O:6].[H-].[Al+3].[Li+].[H-].[H-].[H-].O>O1CCCC1>[OH:6][CH2:5][CH:4]([CH2:3][CH:2]([OH:1])[CH3:15])[CH2:10][OH:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 12000252Diethyl (2-oxopropyl)propanedioateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 22399035HCID 22399035, 화합물수율 100.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 11.4 g of diethyl 2-oxopropylmalonate in 30 ml of tetrahydrofuran was added dropwise under ice-cooling over 20 minutes to a suspension of 5.00 g of lithium aluminum hydride in 100 ml of tetrahydrofuran. The reaction fluid was stirred for an hour under ice-cooling and for 4.5 hours at room temperature, and 10 ml of water was added thereto dropwise under ice-cooling over 20 minutes. The reaction fluid was refluxed for an hour and filtrated. The unfiltered solid was suspended in 200 ml of ethanol and the suspension was refluxed. The suspension was filtrated, and the filtrate combined with the foregoing filtrate was concentrated under a reduced pressure to obtain 7.08 g of 2-hydroxymethyl-1,4-pentanediol as a colorless oily matter.

후처리

  1. temperaturedropwise under ice-cooling over 20 minutes
  2. temperatureThe reaction fluid was refluxed for an hour
  3. filtrationfiltrated
  4. temperaturethe suspension was refluxed
  5. filtrationThe suspension was filtrated
  6. concentrationwas concentrated under a reduced pressure

출처 및 근거

ORD 기록
ord-005b2128d775473da70486ea60378d71
출처 데이터셋
uspto-grants-1995_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05434181

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