Water → 2-[Bis(4-acetoxyphenyl)methyl]-N-(2,4-dimethoxyphenyl)benzamide

HRID 36438

Reaktionsgleichung

Reaktionsgleichung von HRID 36438
[CH3:1][O:2][C:3]1[CH:9]=[C:8]([O:10][CH3:11])[CH:7]=[CH:6][C:4]=1[NH2:5].C(N(CC)CC)C.[C:19]([O:22][C:23]1[CH:28]=[CH:27][C:26]([CH:29]([C:39]2[CH:44]=[CH:43][C:42]([O:45][C:46](=[O:48])[CH3:47])=[CH:41][CH:40]=2)[C:30]2[CH:38]=[CH:37][CH:36]=[CH:35][C:31]=2[C:32](Cl)=[O:33])=[CH:25][CH:24]=1)(=[O:21])[CH3:20].O>C(Cl)Cl>[C:19]([O:22][C:23]1[CH:24]=[CH:25][C:26]([CH:29]([C:39]2[CH:40]=[CH:41][C:42]([O:45][C:46](=[O:48])[CH3:47])=[CH:43][CH:44]=2)[C:30]2[CH:38]=[CH:37][CH:36]=[CH:35][C:31]=2[C:32]([NH:5][C:4]2[CH:6]=[CH:7][C:8]([O:10][CH3:11])=[CH:9][C:3]=2[O:2][CH3:1])=[O:33])=[CH:27][CH:28]=1)(=[O:21])[CH3:20]

Komponenten

6

Edukt 4

HCID 962WaterHCID 8471TriethylamineHCID 176522,4-DimethoxyanilineHCID 152967802-[Bis(4-acetoxyphenyl)methyl]benzoyl chloride

Produkt 1

HCID 152967812-[Bis(4-acetoxyphenyl)methyl]-N-(2,4-dimethoxyphenyl)benzamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

In 20 ml of methylene chloride were dissolved 1.08 g of 2,4-dimethoxyaniline and 4.5 ml of triethylamine. To this solution was dropwise added under ice cooling 20 ml of methylene chloride containing 3 g of 2-[bis(4-acetoxyphenyl)methyl]benzoyl chloride obtained in Reference Example 2. After stirring for 7 hours, water was added thereto. The organic layer was separated off, and the aqueous layer was extracted with chloroform. The chloroform layer was combined with the organic layer, and the combined organic layer was washed with 2N aqueous hydrochloric acid solution and dried over anhydrous magnesium sulfate. The resulting solution was concentrated under reduced pressure to give 2.6 g of the desired product (Compound 2) as an oily matter.

Aufarbeitung

  1. customobtained in Reference Example 2
  2. customThe organic layer was separated off
  3. extractionthe aqueous layer was extracted with chloroform
  4. washthe combined organic layer was washed with 2N aqueous hydrochloric acid solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationThe resulting solution was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-17e1a6fc8d7f4900b476ff014efbe71c
Quelldatensatz
uspto-grants-1995_05
Patentnummer
US05413997

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