Water → N-(2,4-Dichloropyrimidin-5-yl)-4-methoxy-3,5-dimethylbenzamide

HRID 81381ノート

反応式

HRID 81381 の反応式
[NH2:1][C:2]1[C:3]([Cl:9])=[N:4][C:5]([Cl:8])=[N:6][CH:7]=1.C(=O)([O-])O.[Na+].O.[CH3:16][C:17]1[CH:18]=[C:19]([CH:23]=[C:24]([CH3:28])[C:25]=1[O:26][CH3:27])[C:20](Cl)=[O:21]>C(OCC)(=O)C>[Cl:8][C:5]1[N:4]=[C:3]([Cl:9])[C:2]([NH:1][C:20](=[O:21])[C:19]2[CH:23]=[C:24]([CH3:28])[C:25]([O:26][CH3:27])=[C:17]([CH3:16])[CH:18]=2)=[CH:7][N:6]=1

参加物

6

反応物 4

HCID 962WaterHCID 2577975-Amino-2,4-dichloropyrimidineHCID 516892Sodium BicarbonateHCID 214353833,5-Dimethyl-4-methoxybenzoyl chloride

生成物 1

HCID 86675952N-(2,4-Dichloropyrimidin-5-yl)-4-methoxy-3,5-dimethylbenzamide収率 118.5%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 3.2 g of 5-amino-2,4-dichloro-pyrimidine in 50 ml of ethyl acetate was added to a mixture of 25 ml of a saturated aqueous sodium hydrogencarbonate solution and 25 ml of water. A solution of 4.9 g of 3,5-dimethyl-4-methoxy-benzoyl chloride was added at room temperature over a period of 15 min. The mixture was mixed intensively for 4 h. Then the layers were separated and the aqueous layer was extracted twice with ethyl acetate. After drying over sodium sulfate and filtration, the solvent was removed in vacuo to give 7.54 g of raw product. The raw product was triturated with 25 ml of isopropanol. After filtration and washing with 10 ml of isopropanol 2.74 g of the title compound was obtained as a white solid.

後処理

  1. additionThe mixture was mixed intensively for 4 h
  2. customThen the layers were separated
  3. extractionthe aqueous layer was extracted twice with ethyl acetate
  4. dry with materialAfter drying over sodium sulfate and filtration
  5. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-4832a96646f849b39657adba19b1ae56
出典データセット
uspto-grants-2014_09
特許番号
US08846692B2

反応ノート

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