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Ethanol → HCID 178469588, 화합물

HRID 638999
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HRID 638999 반응식
[CH3:1][O:2][C:3]1[CH:9]=[CH:8][C:6]([NH2:7])=[CH:5][CH:4]=1.C([O:12][CH:13]=[C:14]([C:20](OCC)=O)[C:15]([O:17][CH2:18][CH3:19])=[O:16])C.C(O)C>C1C=CC(C2C=CC=CC=2)=CC=1.C1C=CC(OC2C=CC=CC=2)=CC=1>[CH2:18]([O:17][C:15]([C:14]1[CH:20]=[N:7][C:6]2[C:8]([C:13]=1[OH:12])=[CH:9][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)=[O:16])[CH3:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 702EthanolHCID 6871Diethyl (ethoxymethylene)malonateHCID 7732P-Anisidine

생성물 1

HCID 178469588HCID 178469588, 화합물수율 78.9%

시약·촉매·용매 1

HCID 246701,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene)용매

실험 절차

A solution of 4-methoxyaniline (40 g, 0.32 mole) and diethyl ethoxymethylenemalonate (65 mL, 0.32 mole) in Dowtherm A (500 mL) was heated at reflux in a flask fitted with side-arm and condenser, and heating was continued until all the ethanol had distilled off (ca. 0.5 hr). The solution was cooled and pentane was added to give a sticky precipitate. The solvents were decanted off and the residue was treated with more pentane and allowed to stand overnight. The solid was filtered off and washed well with pentane to give the title compound (62.4 g; 78%, contains traces of Dowtherm A).

후처리

  1. temperatureat reflux in a flask
  2. customfitted with side-arm and condenser
  3. temperatureheating
  4. distillationhad distilled off (ca. 0.5 hr)
  5. temperatureThe solution was cooled
  6. additionpentane was added
  7. customto give a sticky precipitate
  8. customThe solvents were decanted off
  9. additionthe residue was treated with more pentane
  10. filtrationThe solid was filtered off
  11. washwashed well with pentane

출처 및 근거

ORD 기록
ord-2bf03c640146472ca5ff1c2b8d06ab99
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07691850B2

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