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

HRID 1937044
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HRID 1937044 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 176
Acetic Acid
용매

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온도
20 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2975d5805cb8435d963c554b3f4f54e5
출처 데이터셋
uspto-grants-2002_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06392050B2

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