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

HRID 472804
ノート
印刷プレビュー

反応式

HRID 472804 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-fbc65bcc32f84804865e03dbdae0407b
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08633223B2

反応ノート

読み込み中…

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