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

HRID 81358ノート

反応式

HRID 81358 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-dichloropyrimidine in 50 ml of ethyl acetate was added to a mixture of 25 ml of a saturated aqueous solution of sodium hydrogencarbonate and 25 ml of water. A solution of 4.9 g of 3,5-dimethyl-4-methoxybenzoyl chloride was added at room temperature over a period of 15 min, and 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 were 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 the solvent
  5. customwas removed in vacuo

出典と根拠

ORDレコード
ord-023e849c215d4f54a839761627eb2f70
出典データセット
uspto-grants-2014_09
特許番号
US08846690B2

反応ノート

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