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Methanol → Ethyl 2-[4-(2-(4-(1-(2-ethoxyethyl)benzimidazole-2-yl)piperidine-1-yl)ethyl)phenyl]-2-methylpropanoate

HRID 384011
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HRID 384011 반응식
[CH2:1]([O:3][C:4](=[O:21])[C:5]([C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH2:15]OS(C)(=O)=O)=[CH:10][CH:9]=1)([CH3:7])[CH3:6])[CH3:2].C(=O)([O-])[O-].[Na+].[Na+].[CH2:28]([O:30][CH2:31][CH2:32][N:33]1[C:37]2[CH:38]=[CH:39][CH:40]=[CH:41][C:36]=2[N:35]=[C:34]1[CH:42]1[CH2:47][CH2:46][NH:45][CH2:44][CH2:43]1)[CH3:29].CO>O>[CH2:1]([O:3][C:4](=[O:21])[C:5]([C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][N:45]2[CH2:46][CH2:47][CH:42]([C:34]3[N:33]([CH2:32][CH2:31][O:30][CH2:28][CH3:29])[C:37]4[CH:38]=[CH:39][CH:40]=[CH:41][C:36]=4[N:35]=3)[CH2:43][CH2:44]2)=[CH:10][CH:9]=1)([CH3:7])[CH3:6])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 887MethanolHCID 10340Sodium CarbonateHCID 138083611-(2-ethoxyethyl)-2-(piperidin-4-yl)-1H-benzo[d]imidazoleHCID 866497982-[4-(2-Methanesulfonyloxy-ethyl)-phenyl]-2-methyl-propionic acid ethylester

생성물 1

HCID 66869688Ethyl 2-[4-(2-(4-(1-(2-ethoxyethyl)benzimidazole-2-yl)piperidine-1-yl)ethyl)phenyl]-2-methylpropanoate수율 90%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

In a reaction vessel, 2-[4-(2-methanesulfonyloxy-ethyl)-phenyl]-2-methyl-propionic acid ethylester (3.2 g) prepared in the Example 8, sodium carbonate (1.1 g), 1-(2-ethoxyethyl)-2-piperidin-4-yl-1H-benzoimidazole (3.0 g) prepared in the Example 12 and methylalcohol (30 mL) were introduced, and the mixture was reacted for 14 hours under reflux condition. Distilled water (50 mL) was added thereto, and the mixture was stirred and crystallized. The crystals were filtered under reduced pressure, and washed with distilled water, and then dried to obtain 2-[4-(2-{4-[1-(2-ethoxy-ethyl)-1H-benzoimidazol-2-yl]-piperidin-1-yl}-ethyl)-phenyl]-2-methyl-propionic acid ethylester (4.5 g, yield 90%, HPLC purity 98.5% or more).

후처리

  1. additionwere introduced
  2. customthe mixture was reacted for 14 hours
  3. temperatureunder reflux condition
  4. customcrystallized
  5. filtrationThe crystals were filtered under reduced pressure
  6. washwashed with distilled water
  7. customdried

출처 및 근거

ORD 기록
ord-0dd6de99bf7142cf8cc38c2ac49bb3d0
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08367704B2

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