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Azane;hydrate → 2-ethyl-1H-pyrrolo[2,3-c]pyridin-5-amine

HRID 513079
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HRID 513079 반응식
[CH2:1]([C:3]1[NH:12][C:6]2=[CH:7][N:8]=[C:9](Cl)[CH:10]=[C:5]2[CH:4]=1)[CH3:2].[NH3:13].O>CCO>[CH2:1]([C:3]1[NH:12][C:6]2=[CH:7][N:8]=[C:9]([NH2:13])[CH:10]=[C:5]2[CH:4]=1)[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 12896473Azane;hydrateHCID 579081942-ethyl-5-chloro-1H-pyrrolo[2,3-c]pyridine

생성물 1

HCID 579081832-ethyl-1H-pyrrolo[2,3-c]pyridin-5-amine수율 16%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
200 °C

실험 절차

A suspension of 2-ethyl-5-chloro-1H-pyrrolo[2,3-c]pyridine (1.3 g, 7.19 mmol) in EtOH (20 mL), CuSO4.5H2O (179 mg, 0.72 mmol) and NH3.H2O (60 ml) was added into an autoclave (100 mL). The reaction was stirred at 200° C. and 2 MPa for 10 h. The reaction was cooled to 25° C. and was quenched with water and extracted with ethyl acetate (100 mL×3). The combined organic layers were dried over anhydrous Na2SO4 and evaporated under reduced pressure. The residue was purified by column chromatography on silica gel (petroleum ether/ethyl acetate, 10/1) to give 2-ethyl-1H-pyrrolo[2,3-c]pyridin-5-amine (190 mg, 16%).

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후처리

  1. additionwas added into an autoclave (100 mL)
  2. temperatureThe reaction was cooled to 25° C.
  3. customwas quenched with water
  4. extractionextracted with ethyl acetate (100 mL×3)
  5. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
  6. customevaporated under reduced pressure
  7. customThe residue was purified by column chromatography on silica gel (petroleum ether/ethyl acetate, 10/1)

출처 및 근거

ORD 기록
ord-49a857d4b2434eadb2e7a4a8f70c74a8
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09102672B2

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