HCID 67431458, 화합물 → HCID 58459125, 화합물

HRID 2036605노트

반응식

HRID 2036605 반응식
[CH:1]1([NH:4][C:5]2[C:14]([N+:15]([O-])=O)=[CH:13][CH:12]=[CH:11][C:6]=2[C:7]([O:9][CH3:10])=[O:8])[CH2:3][CH2:2]1>CO.[Pd]>[NH2:15][C:14]1[C:5]([NH:4][CH:1]2[CH2:3][CH2:2]2)=[C:6]([CH:11]=[CH:12][CH:13]=1)[C:7]([O:9][CH3:10])=[O:8]

참가 물질

4

반응물 1

HCID 67431458HCID 67431458, 화합물

생성물 1

HCID 58459125HCID 58459125, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

To a solution of methyl 2-(cyclopropylamino)-3-nitrobenzoate (1.1 g, 4.5 mmol) in MeOH (4 mL) was added palladium 10 wt % on carbon (0.24 g, 0.23 mmol) under N2. After flushing the flask with N2 several times, the solution was stirred under a H2 balloon for 6 h. LCMS showed the reaction was complete. After filtration of the reaction mixture and rinsing with MeOH, the filtrate was collected and concentrated in vacuo. Purification of the residue by flash chromatography over silica gel column using 0-20% gradient of DCM-MeOH—NH4OH (9:1:0.05) in DCM as eluent gave methyl 3-amino-2-(cyclopropylamino)benzoate: LC-MS (ESI) m/z 207.1 [M+H]+.

후처리

  1. customAfter flushing the flask with N2 several times
  2. filtrationAfter filtration of the reaction mixture
  3. washrinsing with MeOH
  4. customthe filtrate was collected
  5. concentrationconcentrated in vacuo
  6. customPurification of the residue by flash chromatography over silica gel column

출처 및 근거

ORD 기록
ord-27cfdfd3609545469d2ff83e04f2d8bd
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08575183B2

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