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Acetic Acid → Diethyl (2,6-dimethoxybenzylidene)malonate

HRID 326697
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HRID 326697 반응식
[C:1]([O:9][CH2:10][CH3:11])(=[O:8])[CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4].[CH3:12][O:13][C:14]1[CH:21]=[CH:20][CH:19]=[C:18]([O:22][CH3:23])[C:15]=1[CH:16]=O.N1CCCCC1.C(O)(=O)C>O.C1(C)C=CC=CC=1>[CH3:23][O:22][C:18]1[CH:19]=[CH:20][CH:21]=[C:14]([O:13][CH3:12])[C:15]=1[CH:16]=[C:2]([C:3]([O:5][CH2:6][CH3:7])=[O:4])[C:1]([O:9][CH2:10][CH3:11])=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 7761Diethyl MalonateHCID 8082PiperidineHCID 964042,6-Dimethoxybenzaldehyde

생성물 1

HCID 12514881Diethyl (2,6-dimethoxybenzylidene)malonate

시약·촉매·용매 2

HCID 962Water용매
HCID 1140
Toluene
용매

실험 절차

A mixture of 1.52 ml of diethyl malonate, 1.66 g of 2,6-dimethoxybenzaldehyde, 0.1 ml of piperidine, 0.11 ml of glacial acetic acid and 100 ml of toluene was boiled at 110° C. on a water separator for 3.5 hours. The solution was extracted with 10% NaHCO3 solution and back-washed with saturated NaCl solution. The organic phase was dried, filtered under suction and evaporated under reduced pressure. There were obtained 2.8 g of diethyl (2,6-dimethoxybenzylidene)malonate, as a dark yellow oil.

후처리

  1. customfor 3.5 hours
  2. extractionThe solution was extracted with 10% NaHCO3 solution
  3. washback-washed with saturated NaCl solution
  4. customThe organic phase was dried
  5. filtrationfiltered under suction
  6. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-9ac6537c309a41c787eebe8636cabbc8
출처 데이터셋
uspto-grants-1993_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05270313

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