Hydrazine hydrate (1:1) → HCID 19600385、化合物

HRID 609768ノート

反応式

HRID 609768 の反応式
[CH2:1]([N:8]1[C:12]2[CH:13]=[C:14]([Cl:17])[CH:15]=[CH:16][C:11]=2[N:10]=[C:9]1[C:18]([NH:20][C:21]1[CH:22]=[C:23]2[C:27](=[CH:28][CH:29]=1)[N:26]([CH2:30][CH2:31][CH2:32][N:33]1C(=O)C3=CC=CC=C3C1=O)[CH:25]=[CH:24]2)=[O:19])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.NN>C(O)C>[CH2:1]([N:8]1[C:12]2[CH:13]=[C:14]([Cl:17])[CH:15]=[CH:16][C:11]=2[N:10]=[C:9]1[C:18]([NH:20][C:21]1[CH:22]=[C:23]2[C:27](=[CH:28][CH:29]=1)[N:26]([CH2:30][CH2:31][CH2:32][NH2:33])[CH:25]=[CH:24]2)=[O:19])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 19600381HCID 19600381、化合物

生成物 1

HCID 19600385HCID 19600385、化合物収率 82.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To 5 g of 1-benzyl-6-chloro-2-[1-(3-phthalimidopropyl)indol-5-ylaminocarbonyl]benzimidazole was added 100 ml of ethanol and stirred, then 0.5 ml of hydrazine hydrate was added thereto, the mixture was refluxed overnight. After cooled the reaction mixture to room temperature, then white crystals were removed by filtration. Water was added to the filtrate, and made alkaline with 10% aqueous solution of potassium hydroxide. This mixture was extracted with dichloromethane, the extract was washed with water, an aqueous solution saturated with sodium chloride then was dried with anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure. The residue thus obtained was crystallized from ethyl acetate-n-hexane, there was obtained 3.2 g of 1-benzyl-6-chloro-2-[1-(3-aminopropyl)indol-5-ylaminocarbonyl]-benzimidazole as in the form of yellow granular crystals. Melting point: 106-108° C.

後処理

  1. temperaturethe mixture was refluxed overnight
  2. customwhite crystals were removed by filtration
  3. additionWater was added to the filtrate
  4. extractionThis mixture was extracted with dichloromethane
  5. washthe extract was washed with water
  6. dry with materialan aqueous solution saturated with sodium chloride then was dried with anhydrous magnesium sulfate
  7. customThe solvent was removed by distillation under reduced pressure
  8. customThe residue thus obtained
  9. customwas crystallized from ethyl acetate-n-hexane

出典と根拠

ORDレコード
ord-7916107cf1224db786c3f080c25935af
出典データセット
uspto-grants-1999_12
特許番号
US05998437

反応ノート

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