Sodium Hydroxide → 4-{2-[4-(3,3-Dimethyl-butyl)-piperazin-1-yl]-ethoxy}-3-methyl-benzoic Acid

HRID 220845ノート

反応式

HRID 220845 の反応式
C[O:2][C:3](=[O:26])[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH2:11][CH2:12][N:13]2[CH2:18][CH2:17][N:16]([CH2:19][CH2:20][C:21]([CH3:24])([CH3:23])[CH3:22])[CH2:15][CH2:14]2)=[C:6]([CH3:25])[CH:5]=1.[OH-].[Na+]>O1CCOCC1>[CH3:22][C:21]([CH3:24])([CH3:23])[CH2:20][CH2:19][N:16]1[CH2:17][CH2:18][N:13]([CH2:12][CH2:11][O:10][C:7]2[CH:8]=[CH:9][C:4]([C:3]([OH:26])=[O:2])=[CH:5][C:6]=2[CH3:25])[CH2:14][CH2:15]1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 575552114-{2-[4-(3,3-Dimethyl-butyl)-piperazin-1-yl]-ethoxy}-3-methyl-benzoic Acid Methyl Ester

生成物 1

HCID 575552124-{2-[4-(3,3-Dimethyl-butyl)-piperazin-1-yl]-ethoxy}-3-methyl-benzoic Acid収率 100%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

4-{2-[4-(3,3-Dimethyl-butyl)-piperazin-1-yl]-ethoxy}-3-methyl-benzoic acid methyl ester from Example E40.3 (42 mg, 0.12 mmol) was dissolved in dioxan (5 ml) and 1M NaOH (1 ml) was added. The mixture was heated at reflux for 2 h then solvents were concentrated in vacuo. The residue was dissolved in EtOAc, washed with saturated NaHCO3, water then brine, dried and concentrated in vacuo to yield the title compound (40 mg, 100%).

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 2 h
  3. concentrationsolvents were concentrated in vacuo
  4. dissolutionThe residue was dissolved in EtOAc
  5. washwashed with saturated NaHCO3, water
  6. dry with materialbrine, dried
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-5bbdb2fd072b44be97f61975105033dd
出典データセット
uspto-grants-2012_06
特許番号
US08202858B2

反応ノート

読み込み中…