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Acetic Acid → HCID 59323905, 화합물

HRID 1715178
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HRID 1715178 반응식
[N+]([CH:4]([CH3:17])[CH2:5][C:6]1[CH:11]=[CH:10][C:9]([N:12]2[CH:16]=[CH:15][CH:14]=[N:13]2)=[CH:8][CH:7]=1)([O-])=O.C(O)(=[O:20])C>[Fe]>[N:12]1([C:9]2[CH:10]=[CH:11][C:6]([CH2:5][C:4](=[O:20])[CH3:17])=[CH:7][CH:8]=2)[CH:16]=[CH:15][CH:14]=[N:13]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

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HCID 176Acetic Acid2회HCID 68506476HCID 68506476, 화합물

생성물 1

HCID 59323905HCID 59323905, 화합물

시약·촉매·용매 1

HCID 23925Iron촉매

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온도
40 °C

실험 절차

A stirred suspension comprising iron (10.7 g, 191.9 mmol) in glacial acetic acid (150 ml) under an inert atmosphere of argon is heated to 40° C. and then treated with a solution of 1-[4-(2-nitro-propyl)-phenyl]-1H-pyrazole (8.8 g, 38.39 mmol) in glacial acetic acid (100 ml). The reaction mixture is heated to 100° C. for 2 hours and then allowed to cool to room temperature. The mixture is poured onto ice-water (200 ml), stirred for 5 minutes and then filtered through celite washing through with DCM (50 ml). The organic portion of the filtrate is separated and the aqueous is extracted with DCM (150 ml). The organic portions are combined, washed with water (3×50 ml), brine (1×25 ml), dried (MgSO4) and concentrated in vacuo to afford the title compound as a red oil. [MH+ 201.25].

후처리

  1. temperatureThe reaction mixture is heated to 100° C. for 2 hours
  2. temperatureto cool to room temperature
  3. additionThe mixture is poured onto ice-water (200 ml)
  4. filtrationfiltered through celite
  5. washwashing through with DCM (50 ml)
  6. customThe organic portion of the filtrate is separated
  7. extractionthe aqueous is extracted with DCM (150 ml)
  8. washwashed with water (3×50 ml), brine (1×25 ml)
  9. dry with materialdried (MgSO4)
  10. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-ef58223ec3fe4b208c6f83c64779b0b7
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07799810B2

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