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1,3-Dibromopropane → HCID 58123513, 화합물

HRID 536680
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인쇄 미리보기

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HRID 536680 반응식
[CH3:1][O:2][C:3]([CH:5]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7][C:6]1=[O:14])=[O:4].[OH-].[Na+].[Br:17][CH2:18][CH2:19][CH2:20]Br>C(O)C>[CH3:1][O:2][C:3]([C:5]1([CH2:20][CH2:19][CH2:18][Br:17])[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7][C:6]1=[O:14])=[O:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 80011,3-DibromopropaneHCID 14798Sodium HydroxideHCID 10888732Methyl 2-oxo-1-indanecarboxylate

생성물 1

HCID 58123513HCID 58123513, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매2회

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온도
40 °C

실험 절차

A solution of 2-oxo-indan-1-carboxylic acid methyl ester (3.8 g) and NaOH (1 M in water, 20 mL) in ethanol (30 mL) is added dropwise to a solution of 1,3-dibromopropane (10 mL) in ethanol (20 mL) at room temperature. The solution is warmed to 40° C. and stirred at this temperature for 2 d. Then, the solution is concentrated under reduced pressure and ethyl acetate is added to the residue. The resulting mixture is washed with water and brine and dried (MgSO4). After removing the solvent, the residue is purified by chromatography on silica gel (cyclohexane/ethyl acetate 20:1->9:1) to give the title compound as an oil.

후처리

  1. concentrationThen, the solution is concentrated under reduced pressure and ethyl acetate
  2. additionis added to the residue
  3. washThe resulting mixture is washed with water and brine
  4. dry with materialdried (MgSO4)
  5. customAfter removing the solvent
  6. customthe residue is purified by chromatography on silica gel (cyclohexane/ethyl acetate 20:1->9:1)

출처 및 근거

ORD 기록
ord-284a8432efe043d2a89bb5ad579a3d20
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08859580B2

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