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Acetic Acid → Methyl 3-(3,5-dimethoxyphenyl)-2-(4-isopropyloxyphenyl)-3-oxopropionate

HRID 424030
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인쇄 미리보기

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HRID 424030 반응식
[H-].[Na+].[CH3:3][O:4][C:5]1[CH:6]=[C:7]([CH:12]=[C:13]([O:15][CH3:16])[CH:14]=1)[C:8]([O:10]C)=O.[CH:17]([O:20][C:21]1[CH:26]=[CH:25][C:24]([CH2:27][C:28]([O:30][CH3:31])=[O:29])=[CH:23][CH:22]=1)([CH3:19])[CH3:18].C(O)(=O)C>C1(C)C=CC=CC=1.O>[CH3:16][O:15][C:13]1[CH:12]=[C:7]([C:8](=[O:10])[CH:27]([C:24]2[CH:25]=[CH:26][C:21]([O:20][CH:17]([CH3:19])[CH3:18])=[CH:22][CH:23]=2)[C:28]([O:30][CH3:31])=[O:29])[CH:6]=[C:5]([O:4][CH3:3])[CH:14]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 24758Sodium hydrideHCID 75074Methyl 3,5-DimethoxybenzoateHCID 525538Methyl 2-(4-isopropoxyphenyl)acetate

생성물 1

HCID 66674372Methyl 3-(3,5-dimethoxyphenyl)-2-(4-isopropyloxyphenyl)-3-oxopropionate

시약·촉매·용매 2

HCID 962Water
용매
HCID 1140Toluene용매4회

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온도
2.5 °C

실험 절차

14.4 g of 60% sodium hydride in mineral oil (0.36 mol) which are washed with 2 times 50 ml of toluene are introduced into a three-necked round-bottomed flask. 90 ml of toluene and 28.3 g of methyl 3,5-dimethoxybenzoate (0.144 mol) are then introduced. The mixture is brought to reflux and a solution of 30 g of methyl p-isopropyloxyphenylacetate (0.144 mol) dissolved in 95 ml of toluene is added over 10 h. The mixture is maintained at reflux for 2 h. It is cooled to a temperature of 0-5° C. and a solution of glacial acetic acid (22.5 g, i.e. 0.374 mol) in 25 ml of toluene is added slowly. Then, at ambient temperature, 135 ml of water are added slowly.

후처리

  1. additionare introduced into a three-necked round-bottomed flask
  2. temperatureto reflux
  3. additionis added over 10 h
  4. temperatureThe mixture is maintained
  5. temperatureat reflux for 2 h

출처 및 근거

ORD 기록
ord-f134aec402f947f3b6994412ef96e865
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08101804B2

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