Hydrochloric Acid → HCID 20135762、化合物

HRID 484868ノート

反応式

HRID 484868 の反応式
[CH2:1]([N:3]([CH2:23][CH3:24])[CH2:4][CH2:5][CH2:6][NH:7][C:8]1[C:16]2[C:11](=[C:12]([N+:20]([O-])=O)[CH:13]=[C:14]([N+:17]([O-])=O)[CH:15]=2)[NH:10][N:9]=1)[CH3:2].CO.O.Cl>[Fe].C(Cl)(Cl)Cl>[CH2:23]([N:3]([CH2:1][CH3:2])[CH2:4][CH2:5][CH2:6][NH:7][C:8]1[C:16]2[C:11](=[C:12]([NH2:20])[CH:13]=[C:14]([NH2:17])[CH:15]=2)[NH:10][N:9]=1)[CH3:24]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 962WaterHCID 20135777N~3~-(5,7-Dinitro-1H-indazol-3-yl)-N~1~,N~1~-diethylpropane-1,3-diamine

生成物 1

HCID 20135762HCID 20135762、化合物収率 22.6%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 6212Chloroform溶媒

反応条件

温度
70 °C

実験手順

A mixture consisting of 9.0 g of the 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. The ethyl acetate layer was washed with water and dried over anhydrous sodium sulfate. Then, 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 1.67 g of 3-(3-diethylaminopropylamino)-5,7-diaminoindazole having the following analytical values in a yield of 22%.

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 materialdried over anhydrous sodium sulfate
  6. customThen, ethyl acetate was removed under reduced pressure
  7. customThe residue thus obtained

出典と根拠

ORDレコード
ord-2c4e3818584b4a9499436ad7252c81e0
出典データセット
uspto-grants-1985_08
特許番号
US04533731

反応ノート

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