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

HRID 220845노트

반응식

HRID 220845 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-5bbdb2fd072b44be97f61975105033dd
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08202858B2

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