Sodium Hydroxide → HCID 178464037、化合物

HRID 1390022

反応式

HRID 1390022 の反応式
[CH2:1]([N:3]([CH2:17][CH3:18])[CH2:4][CH2:5][N:6]1[C:10]2[N:11]=[C:12]([Cl:15])[CH:13]=[CH:14][C:9]=2[N:8]=[C:7]1[OH:16])[CH3:2].[Cl:19]([O-])(=O)=O.[K+].[OH-].[Na+]>Cl>[CH2:17]([N:3]([CH2:1][CH3:2])[CH2:4][CH2:5][N:6]1[C:10]2[N:11]=[C:12]([Cl:15])[C:13]([Cl:19])=[CH:14][C:9]=2[N:8]=[C:7]1[OH:16])[CH3:18]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 6426889Potassium ChlorateHCID 178464036HCID 178464036、化合物

生成物 1

HCID 178464037HCID 178464037、化合物

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

反応条件

温度
33 °C

実験手順

15 grams of 1-(2-diethylaminoethyl)-2-hydroxy-6-chloro-7-aza-benzimidazole were dissolved in 200 ml of concentrated hydrochloric acid and there were added in portions with stirring 24.5 grams of potassium chlorate at room temperature. The temperature increased temporarily to 33° C. The mixture was stirred for another hour, made alkaline with sodium hydroxide, the mixture extracted with shaking with n-butanol, the extract evaporated in a vacuum and the residue chromatographed over silica gel. The reaction product was recrystallized from ethyl acetate. M.P. 137°-139° C.; Yield: 3 grams.

後処理

  1. additionthere were added in portions
  2. extractionthe mixture extracted
  3. stirringwith shaking with n-butanol
  4. customthe extract evaporated in a vacuum
  5. customthe residue chromatographed over silica gel
  6. customThe reaction product was recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-b3af77507a9447b2b79d28e48f76a33f
出典データセット
uspto-grants-1981_01
特許番号
US04247556

関連ノート

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