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Benzaldehyde → Methyl 2-(1-oxopropyl)-3-(4-fluorophenyl)-4-phenyl-4-oxobutanoate

HRID 2107087
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HRID 2107087 반응식
[F:1][C:2]1[CH:17]=[CH:16][C:5]([CH:6]=[C:7]([C:12](=[O:15])[CH2:13][CH3:14])[C:8]([O:10][CH3:11])=[O:9])=[CH:4][CH:3]=1.[CH:18](=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.C(N(CC)CC)C.C(O)C>[I-].C[N+]1C(C)=C(CCO)SC=1.ClCCl>[O:15]=[C:12]([CH:7]([CH:6]([C:5]1[CH:4]=[CH:3][C:2]([F:1])=[CH:17][CH:16]=1)[C:18]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[O:25])[C:8]([O:10][CH3:11])=[O:9])[CH2:13][CH3:14]
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참가 물질

7

반응물 4

HCID 240BenzaldehydeHCID 702EthanolHCID 8471TriethylamineHCID 53755005Methyl 2-(4-fluorobenzylidene)-3-oxopentanoate

생성물 1

HCID 23047461Methyl 2-(1-oxopropyl)-3-(4-fluorophenyl)-4-phenyl-4-oxobutanoate수율 28.5%

시약·촉매·용매 2

HCID 9838770
3,4-Dimethyl-5-(2-hydroxyethyl)thiazolium iodide
촉매
HCID 6344Dichloromethane용매

실험 절차

A mixture of methyl 2-(4-fluorobenzylidene)-3-oxopentanoate (52.0 g), benzaldehyde (25.4 g), triethylamine (22 g), 3,4-dimethyl-5-(2-hydroxyethyl)thiazolium iodide (6.3 g) and ethanol (100 ml) was heated at reflux under nitrogen for 16 hours. The cooled mixture was diluted with dichloromethane, and washed with dilute hydrochloric acid (2N), with dilute aqueous sodium bicarbonate solution, and with water, and dried over magnesium sulphate. The solution was concentrated in vacuo and the residue was dissolved in hot methanol. The resulting off-white solid was filtered off, to give methyl 2-(1-oxopropyl)-3-(4-fluorophenyl)-4-phenyl-4-oxobutanoate (21.5 g), m.p. 104°-109° C. [Elemental analysis: C,70.1;H,5.42;F,5.58%; calculated: C,70.15;H,5.60; F,5.55%; I.R. 1749, 1738, 1716, 1708, 1679, 1508, 761, 697cm-1 [N.M.R. (in CDCl3): 0.81 and 1.08 (3H, two triplets, J=7 Hz), 1.80-2.04 and 2.46-2.80 (2H, two sets of multiplets), 3.53 and 3.68 (3H, two singlets), 4.58 and 4.62 (1H, two doublets, J=10 Hz), 5.39 and 5.42 (1H, two doublets, J=10 Hz), 6.96 (2H, t, J=8 Hz), 7.20- 7.60 (5H, m), 7.90-8.00 (2H, m)].

후처리

  1. temperaturewas heated
  2. temperatureat reflux under nitrogen for 16 hours
  3. washwashed with dilute hydrochloric acid (2N), with dilute aqueous sodium bicarbonate solution
  4. dry with materialwith water, and dried over magnesium sulphate
  5. concentrationThe solution was concentrated in vacuo
  6. dissolutionthe residue was dissolved in hot methanol
  7. filtrationThe resulting off-white solid was filtered off

출처 및 근거

ORD 기록
ord-64489adf48f149e6a120ce7a2bd1f8c2
출처 데이터셋
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04933350

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