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Water → Dimethyl 2,6-diisopropyl-4-(4-fluorophenyl)-pyridine-3,5-dicarboxylate

HRID 1937044
ノート
印刷プレビュー

反応式

HRID 1937044 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[C:13]([C:14]([O:16][CH3:17])=[O:15])=[C:12]([CH:18]([CH3:20])[CH3:19])[NH:11][C:10]([CH:21]([CH3:23])[CH3:22])=[C:9]2[C:24]([O:26][CH3:27])=[O:25])=[CH:4][CH:3]=1.O.N(OC)=O.[OH-].[Na+]>C(O)(=O)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:9]([C:24]([O:26][CH3:27])=[O:25])=[C:10]([CH:21]([CH3:22])[CH3:23])[N:11]=[C:12]([CH:18]([CH3:19])[CH3:20])[C:13]=2[C:14]([O:16][CH3:17])=[O:15])=[CH:6][CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 12231Methyl nitriteHCID 14798Sodium HydroxideHCID 11199700DIMETHYL 1,4-DIHYDRO-2,6-DIISOPROPYL-4-(4-FLUOROPHENYL)-PYRIDINE-3,5-DICARBOXYLATE

生成物 1

HCID 9969567Dimethyl 2,6-diisopropyl-4-(4-fluorophenyl)-pyridine-3,5-dicarboxylate収率 95%

試薬・触媒・溶媒 1

HCID 176
Acetic Acid
溶媒

反応条件

温度
20 °C

実験手順

In a 4 1 glass reactor, 750 g 4-(4-fluorophenyl)-2,6-diisopropyl-3,5-di(methoxy-carbonyl)-1,4-dihydropyridine were mixed with 2250 g water and 245 g of acetic acid. Thereafter 7 mols of methyl nitrite were introduced at 58 to 60° C. After cooling to 20° C. 363 g of 45% by weight strength aqueous sodium hydroxide were added to result in an increase of the pH up to 9. The resulting suspension was filtered and the product that has been filtered off was washed twice with in each case 800 ml of water and then dried at 50 to 60° C. under reduced pressure. 708 g of 4-(4-fluoropheny) -2,6-diisopropyl-3,5-di(methoxy-carbonyl)-pyridine were isolated, which corresponds to a yield of 95% of theory.

後処理

  1. customto result in
  2. temperaturean increase of the pH up to 9
  3. filtrationThe resulting suspension was filtered
  4. filtrationthe product that has been filtered off
  5. washwas washed twice with in each case 800 ml of water
  6. customdried at 50 to 60° C. under reduced pressure

出典と根拠

ORDレコード
ord-2975d5805cb8435d963c554b3f4f54e5
出典データセット
uspto-grants-2002_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06392050B2

反応ノート

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