Sodium Hydroxide → HCID 23156137、化合物

HRID 1890651ノート

反応式

HRID 1890651 の反応式
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][NH:15][C:16]2[CH:21]=[CH:20][C:19]([CH2:22][N:23]3[C:27]4=[N:28][C:29]([CH3:33])=[CH:30][C:31]([CH3:32])=[C:26]4[N:25]=[C:24]3[CH3:34])=[CH:18][CH:17]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.C(OCC)(=O)C.Cl.[OH-].[Na+]>C(Cl)(Cl)Cl>[CH3:34][C:24]1[N:23]([CH2:22][C:19]2[CH:20]=[CH:21][C:16]([NH:15][CH2:14][CH:11]3[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]3)=[CH:17][CH:18]=2)[C:27]2=[N:28][C:29]([CH3:33])=[CH:30][C:31]([CH3:32])=[C:26]2[N:25]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 21866389Hydrogen chloride-ethyl acetateHCID 694347614-[4-(2,5,7-trimethyl-3H-imidazo[4,5-b]pyridin-3-ylmethyl)phenylamino]methylpiperidine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 23156137HCID 23156137、化合物収率 99.7%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A solution of 4-[4-(2,5,7-trimethyl-3H-imidazo[4,5-b]pyridin-3-ylmethyl)phenylamino]methylpiperidine-1-carboxylic acid tert-butyl ester (1.53 g, 3.31 mmol) obtained in Step 1 in chloroform (15 mL) was added with a 4 mol/L hydrogen chloride-ethyl acetate solution (7.0 mL) followed by stirring at room temperature for 2 hours. The reaction mixture was added with a 2 mol/L aqueous sodium hydroxide solution to control the pH to 12, and extracted with chloroform three times. The organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain Compound 157 (1.20 g, 3.3 mmol, 99%).

後処理

  1. extractionextracted with chloroform three times
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-860f8774b38e441f8d38e18cf71ce779
出典データセット
uspto-grants-2013_08
特許番号
US08507484B2

反応ノート

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