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Hydrochloric Acid → HCID 20135876、化合物

HRID 484896
ノート
印刷プレビュー

反応式

HRID 484896 の反応式
[CH2:1]([N:3]([CH2:31][CH3:32])[CH2:4][CH2:5][CH2:6][N:7]1[C:15]2[C:10](=[CH:11][C:12]([N+:19]([O-])=O)=[CH:13][C:14]=2[N+:16]([O-])=O)[C:9]([NH:22][CH2:23][CH2:24][CH2:25][N:26]([CH2:29][CH3:30])[CH2:27][CH3:28])=[N:8]1)[CH3:2].CO.O.Cl>[Fe].C(Cl)(Cl)Cl>[CH2:31]([N:3]([CH2:1][CH3:2])[CH2:4][CH2:5][CH2:6][N:7]1[C:15]2[C:10](=[CH:11][C:12]([NH2:19])=[CH:13][C:14]=2[NH2:16])[C:9]([NH:22][CH2:23][CH2:24][CH2:25][N:26]([CH2:27][CH3:28])[CH2:29][CH3:30])=[N:8]1)[CH3:32]
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

7

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 962WaterHCID 20135767HCID 20135767、化合物

生成物 1

HCID 20135876HCID 20135876、化合物収率 23.7%

試薬・触媒・溶媒 2

HCID 23925Iron触媒
HCID 6212
Chloroform
溶媒

反応条件

温度
70 °C

実験手順

A mixture consisting of 12.0 g of the 1-(3-diethylaminopropyl)-3-(3-diethylaminopropylamino)-5,7-dinitroindazole, 18 g of iron powder, 60 ml of methyl alcohol, 30 ml of water and 3 ml of hydrochloric acid was stirred for 1.5 hours at 70° C. After cooling, the mixture was filtered, and the pH of the filtrate was adjusted to 11 with an aqueous potassium carbonate solution. The filtrate was extracted three times with 50 ml of ethyl acetate, and the ethyl acetate layer was washed with water. The layer was dried over anhydrous sodium sulfate, and ethyl acetate was removed under reduced pressure. The residue thus obtained was subjected to an alumina-column chromatography (alumina: 200 g) using chloroform as the developing solvent to give 2.46 g of 1-(3-diethylaminopropyl)-3-(3-diethylaminopropylamino)-5,7-diaminoindazole having the following analytical values in a yield of 23%.

後処理

  1. temperatureAfter cooling
  2. filtrationthe mixture was filtered
  3. extractionThe filtrate was extracted three times with 50 ml of ethyl acetate
  4. washthe ethyl acetate layer was washed with water
  5. dry with materialThe layer was dried over anhydrous sodium sulfate, and ethyl acetate
  6. customwas removed under reduced pressure
  7. customThe residue thus obtained

出典と根拠

ORDレコード
ord-b5efbfb913a5466185b4fe07023694ee
出典データセット
uspto-grants-1985_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04533731

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート