反応 #70342

ord-ae17b7f92e9047fa9b704095ee8458a9

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過After that the reaction mixture was filtered
  2. 2
    濃縮concentrated
  3. 3
    workup.DISSOLUTIONredissolved in water
  4. 4
    workup.ADDITIONThe pH was adjusted to 4-5 by addition of 2N NaOH
  5. 5
    その他a solid was formed
  6. 6
    その他This yellow solid formed

実験手順

A solution of 5-methyl-2-(quinolin-3-ylamino)benzoic acid (Example 16) (1.08 mmol, 0.30 g) in TFA (2.5 ml) was hydrogenated under pressure (58 psi) with PtO2 (0.11 mmol, 0.028 g) as catalyst until all starting material disappeared. After that the reaction mixture was filtered, concentrated and redissolved in water. The pH was adjusted to 4-5 by addition of 2N NaOH and a solid was formed. This yellow solid formed was the desired compound (0.249 mg, 79% of yield).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08536165B2uspto-grants-2013_09