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

HRID 1709655
ノート
印刷プレビュー

反応式

HRID 1709655 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6604b154d7244ec88f154bba03a606ed
出典データセット
uspto-grants-1990_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04950675

反応ノート

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