HCID 67431458、化合物 → HCID 58459125、化合物

HRID 2036605ノート

反応式

HRID 2036605 の反応式
[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]

参加物

4

反応物 1

HCID 67431458HCID 67431458、化合物

生成物 1

HCID 58459125HCID 58459125、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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]+.

後処理

  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

出典と根拠

ORDレコード
ord-27cfdfd3609545469d2ff83e04f2d8bd
出典データセット
uspto-grants-2013_11
特許番号
US08575183B2

反応ノート

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