Sodium Hydroxide → HCID 178464037, 화합물

HRID 1390022

반응식

HRID 1390022 반응식
[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]

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 6426889Potassium ChlorateHCID 178464036HCID 178464036, 화합물

생성물 1

HCID 178464037HCID 178464037, 화합물

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

반응 조건

온도
33 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b3af77507a9447b2b79d28e48f76a33f
출처 데이터셋
uspto-grants-1981_01
특허 번호
US04247556

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