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Ammonium Hydroxide → DIMETHYL 1,4-DIHYDRO-2,6-DIISOPROPYL-4-(4-FLUOROPHENYL)-PYRIDINE-3,5-DICARBOXYLATE

HRID 1709655
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HRID 1709655 반응식
[CH3:1][O:2][C:3](=[O:10])[CH2:4][C:5](=O)[CH:6]([CH3:8])[CH3:7].[F:11][C:12]1[CH:19]=[CH:18][C:15]([CH:16]=O)=[CH:14][CH:13]=1.[OH-:20].[NH4+:21]>CO>[C:3]([C:4]1[CH:16]([C:15]2[CH:18]=[CH:19][C:12]([F:11])=[CH:13][CH:14]=2)[C:4]([C:3]([O:2][CH3:1])=[O:20])=[C:5]([CH:6]([CH3:8])[CH3:7])[NH:21][C:5]=1[CH:6]([CH3:8])[CH3:7])([O:2][CH3:1])=[O:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14923Ammonium HydroxideHCID 680234-FluorobenzaldehydeHCID 2759969Methyl 4-methyl-3-oxopentanoate

생성물 1

HCID 11199700DIMETHYL 1,4-DIHYDRO-2,6-DIISOPROPYL-4-(4-FLUOROPHENYL)-PYRIDINE-3,5-DICARBOXYLATE

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 152 g (1.05 mole) 4-methyl-3-oxopentanic acid methyl ester, 56 ml (1.05 mole) 4-fluoro benzaldehyde and 40 ml conc. ammonium hydroxide was heated to reflux in 200 ml methanol for 48 hours. The reaction mixture was then concentrated in vacuo, the viscous residue was dissolved in 500 ml ethylether and washed with saturated sodium bisulfite. The organic layer was dried over magnesium sulfate, filtered and evaporated to yield 202 g of the Step 1 title product. Analysis for C21H26FNO4. calc; C, 67.18; H, 6.98; N, 3,73. Found: C, 67.40; H, 7.48; N, 3.88.

후처리

  1. temperaturewas heated
  2. concentrationThe reaction mixture was then concentrated in vacuo
  3. dissolutionthe viscous residue was dissolved in 500 ml ethylether
  4. washwashed with saturated sodium bisulfite
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated

출처 및 근거

ORD 기록
ord-6604b154d7244ec88f154bba03a606ed
출처 데이터셋
uspto-grants-1990_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04950675

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