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Ammonium formate → 2-isopropoxypyridin-3-amine

HRID 450561
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HRID 450561 반응식
[CH:1]([O:4][C:5]1[C:10]([N+:11]([O-])=O)=[CH:9][CH:8]=[CH:7][N:6]=1)([CH3:3])[CH3:2].C([O-])=O.[NH4+]>C(O)C.[OH-].[OH-].[Pd+2]>[CH:1]([O:4][C:5]1[C:10]([NH2:11])=[CH:9][CH:8]=[CH:7][N:6]=1)([CH3:3])[CH3:2]
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참가 물질

5

반응물 2

HCID 2723923Ammonium formateHCID 696692682-(1-Methylethoxy)-3-nitropyridine

생성물 1

HCID 218508472-isopropoxypyridin-3-amine

시약·촉매·용매 2

HCID 9942167Palladium hydroxide촉매HCID 702Ethanol용매

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온도
90 °C

실험 절차

Palladium hydroxide on carbon (20%, 0.076 g, 0.54 mmol) was added into a solution of 2-iso-propoxy-3-nitro-pyridine (1.97 g, 10.8 mmol) and ammonium formate (3.40 g, 54.0 mmol) in ethanol (100 mL) at ambient temperature. The solution was stirred for 2 hours at 90° C., cooled to ambient temperature, filtered through Celite and washed with MeOH. The filtrate was concentrated in vacuo and triturated from diethyl ether to yield brown oil which was used in the next step without further purification.

후처리

  1. temperaturecooled to ambient temperature
  2. filtrationfiltered through Celite
  3. washwashed with MeOH
  4. concentrationThe filtrate was concentrated in vacuo
  5. customtriturated from diethyl ether
  6. customto yield brown oil which
  7. customwas used in the next step without further purification

출처 및 근거

ORD 기록
ord-38b385b86d064a22905507dafa8eb245
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08486953B2

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