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Phosphoric Acid → HCID 178428356、化合物

HRID 488001
ノート
印刷プレビュー

反応式

HRID 488001 の反応式
[CH:1]1([C:4](O)=O)[CH2:3][CH2:2]1.P(=O)(O)(O)O.[NH2:12][C:13]1[C:18]([NH2:19])=[C:17]([CH3:20])[CH:16]=[CH:15][N:14]=1.[OH-].[K+]>O>[CH:1]1([C:4]2[NH:12][C:13]3=[N:14][CH:15]=[CH:16][C:17]([CH3:20])=[C:18]3[N:19]=2)[CH2:3][CH2:2]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 1004Phosphoric AcidHCID 14797Potassium HydroxideHCID 15655Cyclopropanecarboxylic acidHCID 3174954-Methylpyridine-2,3-diamine

生成物 1

HCID 178428356HCID 178428356、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
130 °C

実験手順

30 ml of cyclopropanecarboxylic acid and 70 ml of phosphoric acid (85%) were added to 15 g of 2,3-diamino-4-methylpyridine, and the mixture was stirred at an internal temperature of 130° C. for 12 hr. The reaction mixture was cooled, poured into a solution of 140 g of potassium hydroxide in 420 ml of water and then extracted with chloroform. The extract was dried over anhydrous magnesium sulfate and then concentrated. The residue was purified by column chromatography (chloroform:ethanol=97:3). The yield was 14.1 g, and the product was recrystallized from ethyl acetate-isopropyl ether to prepare the title compound in a pure form having a melting point of 203° to 204° C.

後処理

  1. temperatureThe reaction mixture was cooled
  2. extractionextracted with chloroform
  3. dry with materialThe extract was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified by column chromatography (chloroform:ethanol=97:3)
  6. customThe yield was 14.1 g, and the product was recrystallized from ethyl acetate-isopropyl ether
  7. customto prepare the title compound in a pure form

出典と根拠

ORDレコード
ord-e27f96153f724710a8374fa4052780b3
出典データセット
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05298518

反応ノート

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