Hydrochloric Acid → HCID 12640243、化合物

HRID 1680457ノート

反応式

HRID 1680457 の反応式
[F:1][C:2]1[CH:18]=[CH:17][C:5]([CH2:6][NH:7][C:8]2[CH:9]=[CH:10][C:11]([C:14]([OH:16])=[O:15])=[N:12][CH:13]=2)=[CH:4][CH:3]=1.C(OO)(=[O:21])C.Cl>O.[OH-].[Na+]>[F:1][C:2]1[CH:18]=[CH:17][C:5]([CH2:6][NH:7][C:8]2[CH:13]=[N+:12]([O-:21])[C:11]([C:14]([OH:16])=[O:15])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 6585Peracetic Acid2 回HCID 126401915-{[(4-Fluorophenyl)methyl]amino}pyridine-2-carboxylic acid

生成物 1

HCID 12640243HCID 12640243、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

5.77 g of 5-(p-fluorobenzylamino)-pyridine-2-carboxylic acid are dissolved in 40 ml of water and 20 ml of 2 N aqueous sodium hydroxide. The solution is stirred at room temperature and 3.6 g of 40% aqueous peracetic acid are added. The solution becomes green and within less than a minute a solid separates. Another 3.6 g of said peracetic acid are added and the mixture is stirred for 4 hours. The pH of the mixture is adjusted to 4 with hydrochloric acid and filtered after cooling. The solid is collected and recrystallized from 90% aqueous acetonitrile, to yield the 5-(p-fluorobenzylamino)-pyridine-2-carboxylic acid N-oxide melting at 206°-209°.

後処理

  1. stirringthe mixture is stirred for 4 hours
  2. filtrationfiltered
  3. temperatureafter cooling
  4. customThe solid is collected
  5. customrecrystallized from 90% aqueous acetonitrile

出典と根拠

ORDレコード
ord-a576b0cbc33843b482784f84646db573
出典データセット
uspto-grants-1981_06
特許番号
US04273779

反応ノート

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