Hydrochloric Acid → HCID 20135762, 화합물

HRID 484868노트

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HRID 484868 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 20135762HCID 20135762, 화합물수율 22.6%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 6212Chloroform용매

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온도
70 °C

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-2c4e3818584b4a9499436ad7252c81e0
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04533731

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