Sodium Hydroxide → HCID 178512998、化合物

HRID 2119027ノート

反応式

HRID 2119027 の反応式
Cl.[C:2]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[NH:11][C:12]([C@H:14]1[CH2:19][CH2:18][C@H:17]([CH2:20][NH:21][C:22]([NH2:24])=[NH:23])[CH2:16][CH2:15]1)=[O:13])([OH:4])=[O:3].[OH-].[Na+]>CO.O>[C:2]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[NH:11][C:12]([C@H:14]1[CH2:15][CH2:16][C@H:17]([CH2:20][NH:21][C:22]([NH2:24])=[NH:23])[CH2:18][CH2:19]1)=[O:13])([OH:4])=[O:3]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 178479469HCID 178479469、化合物

生成物 1

HCID 178512998HCID 178512998、化合物収率 60.4%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

The N-(o-carboxyphenyl)-trans-4-guanidinomethylcyclohexanecarboxamide hydrochloride (5.0 g, 0.013 mole) obtained above is dissolved in methanol (30 ml) and the mixture is added under ice-cooling to a solution of NaOH (3.25 g, 0.0813 mole) in water (10 ml), and the mixture is stirred under ice-cooling for 30 minutes and further stirred at room temperature for 2 hours. The resulting precipitates are taken by filtration and dissolved in acetic acid (50 ml). After evaporation of the solvent under reduced pressure, the residue is washed with methanol and recrystallized from acetic acid-water to give N-(o-carboxyphenyl)trans-4-guanidinomethylcyclohexanecarboxamide (2.5 g). m.p. 300°-310° C. (decomp.)

後処理

  1. additionthe mixture is added under ice-
  2. temperaturecooling for 30 minutes
  3. stirringfurther stirred at room temperature for 2 hours
  4. customThe resulting precipitates
  5. filtrationare taken by filtration
  6. dissolutiondissolved in acetic acid (50 ml)
  7. customAfter evaporation of the solvent under reduced pressure
  8. washthe residue is washed with methanol
  9. customrecrystallized from acetic acid-water

出典と根拠

ORDレコード
ord-8f6815a203bb45faa26b2daa0ce42e74
出典データセット
uspto-grants-1987_07
特許番号
US04681895

反応ノート

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