Nitrogen → HCID 67958057, 화합물

HRID 82836노트

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HRID 82836 반응식
N#N.[CH3:3][O:4][C:5]([C:8]1[N:9]=[C:10]([CH2:13][N:14]2[N:18]=[C:17]([N+:19]([O-])=O)[CH:16]=[N:15]2)[O:11][CH:12]=1)([CH3:7])[CH3:6].[NH4+].[Cl-]>CCO.O.[Fe]>[CH3:3][O:4][C:5]([C:8]1[N:9]=[C:10]([CH2:13][N:14]2[N:18]=[C:17]([NH2:19])[CH:16]=[N:15]2)[O:11][CH:12]=1)([CH3:7])[CH3:6]

참가 물질

7

반응물 3

HCID 947NitrogenHCID 25517Ammonium ChlorideHCID 679582554-(2-Methoxypropan-2-yl)-2-((4-nitro-2H-1,2,3-triazol-2-yl)methyl)oxazole

생성물 1

HCID 67958057HCID 67958057, 화합물

시약·촉매·용매 3

HCID 23925Iron촉매HCID 702Ethanol용매HCID 962Water용매

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온도
85 °C

실험 절차

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a mixture of 4-(2-methoxypropan-2-yl)-2-((4-nitro-2H-1,2,3-triazol-2-yl)methyl)oxazole (56 mg, 0.21 mmol), iron powder (35 mg, 0.63 mmol) and NH4Cl (57 mg, 1.05 mmol) in a mixture of EtOH (1.0 mL) and water (0.5 mL) was stirred at 85° C. for 15 min. The reaction mixture was filtered while hot and concentrated under reduced pressure. CH2Cl2 (2 mL) was added followed by 1N NaOH (2 mL). The layers were separated and the aq. layer was extracted with CH2Cl2 (2 mL). The combined org. extracts were dried over MgSO4, filtered, and the solvents were removed under reduced pressure to give the title compound as a yellow oil. LC-MS-conditions 06: tR=0.46 min; [M+H]+=238.09.

후처리

  1. filtrationThe reaction mixture was filtered while hot and
  2. concentrationconcentrated under reduced pressure
  3. additionCH2Cl2 (2 mL) was added
  4. customThe layers were separated
  5. extractionthe aq. layer was extracted with CH2Cl2 (2 mL)
  6. dry with materialextracts were dried over MgSO4
  7. filtrationfiltered
  8. customthe solvents were removed under reduced pressure

출처 및 근거

ORD 기록
ord-3162d9768d0b46549ee84e51212d4e88
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846733B2

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