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Hydrochloric Acid → HCID 20135876, 화합물

HRID 484896
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인쇄 미리보기

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HRID 484896 반응식
[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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 962WaterHCID 20135767HCID 20135767, 화합물

생성물 1

HCID 20135876HCID 20135876, 화합물수율 23.7%

시약·촉매·용매 2

HCID 23925Iron촉매
HCID 6212
Chloroform
용매

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온도
70 °C

실험 절차

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%.

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 materialThe layer was dried over anhydrous sodium sulfate, and ethyl acetate
  6. customwas removed under reduced pressure
  7. customThe residue thus obtained

출처 및 근거

ORD 기록
ord-b5efbfb913a5466185b4fe07023694ee
출처 데이터셋
uspto-grants-1985_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04533731

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