4-Fluorobenzaldehyde → 3-Methyl 5-ethyl 1,4-dihydro-2,4-di-(4-fluorophenyl)-6-isopropylpyridine-3,5-di-carboxylate

HRID 582556

반응식

HRID 582556 반응식
[F:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=O)=[CH:4][CH:3]=1.[F:10][C:11]1[CH:23]=[CH:22][C:14]([C:15]([CH2:17][C:18]([O:20][CH3:21])=[O:19])=O)=[CH:13][CH:12]=1.[NH2:24][C:25]([CH:32]([CH3:34])[CH3:33])=[CH:26][C:27]([O:29][CH2:30][CH3:31])=[O:28]>C(O)CO>[F:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]2[NH:24][C:25]([CH:32]([CH3:33])[CH3:34])=[C:26]([C:27]([O:29][CH2:30][CH3:31])=[O:28])[CH:15]([C:14]3[CH:13]=[CH:12][C:11]([F:10])=[CH:23][CH:22]=3)[C:17]=2[C:18]([O:20][CH3:21])=[O:19])=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 680234-FluorobenzaldehydeHCID 579425Methyl 4-fluorobenzoylacetateHCID 59557418Ethyl 3-amino-4-methyl-pent-2-enoate

생성물 1

HCID 158172683-Methyl 5-ethyl 1,4-dihydro-2,4-di-(4-fluorophenyl)-6-isopropylpyridine-3,5-di-carboxylate

시약·촉매·용매 1

HCID 174Ethylene Glycol용매

실험 절차

31 g (0.25 mol) of p-fluorobenzaldehyde, 49 g (0.25 mol) of methyl 4-fluorobenzoylacetate and 39.25 g (0.25 mol) of ethyl 3-amino-4-methyl-pent-2-enoate are boiled under reflux for 18 hours in 150 ml of ethylene glycol at a bath temperature of 130° C. The mixture is cooled to room temperature, extracted three times using 300 ml of diethyl ether, the combined ether phases are concentrated, and the residue is dissolved in 100 ml of toluene and chromatographed on 700 ml of silica gel (0.04-0.063 mm) using toluene as an eluent.

후처리

  1. extractionextracted three times
  2. concentrationthe combined ether phases are concentrated
  3. dissolutionthe residue is dissolved in 100 ml of toluene
  4. customchromatographed on 700 ml of silica gel (0.04-0.063 mm)

출처 및 근거

ORD 기록
ord-1cf92cccaaf44470a769683b290a9484
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05925645

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