Sodium Bicarbonate → HCID 57642825、化合物

HRID 2112908ノート

反応式

HRID 2112908 の反応式
C([O-])(=[O:3])C.[Na+].C(=O)(O)[O-].[Na+].[C:11]([O:15][C:16]([N:18]1[CH2:23][CH2:22][N:21]([C:24]2[N:32]=[CH:31][N:30]=[C:29]3[C:25]=2[N:26]=[C:27](Cl)[N:28]3[CH2:33][C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][C:35]=2[C:40]#[N:41])[CH2:20][CH2:19]1)=[O:17])([CH3:14])([CH3:13])[CH3:12]>CS(C)=O>[C:11]([O:15][C:16]([N:18]1[CH2:23][CH2:22][N:21]([C:24]2[N:32]=[CH:31][N:30]=[C:29]3[C:25]=2[NH:26][C:27](=[O:3])[N:28]3[CH2:33][C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][C:35]=2[C:40]#[N:41])[CH2:20][CH2:19]1)=[O:17])([CH3:14])([CH3:13])[CH3:12]

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 517045Sodium AcetateHCID 57642834HCID 57642834、化合物

生成物 1

HCID 57642825HCID 57642825、化合物収率 45.9%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
135 °C

実験手順

Sodium acetate (0.168 g) and sodium bicarbonate (0.100 g) were added to a solution of 4-[8-chloro-9-(2-cyanobenzyl)-9H-purin-6-yl]-piperazine-1-carboxylic acid t-butyl ester (0.100 g) in dimethylsulfoxide (3 mL). This was then heated at 135° C. for 45 hours. The reaction solution was filtered, and then directly loaded onto a column for purification by reverse phase high performance liquid chromatography to give the title compound (0.044 g).

後処理

  1. filtrationThe reaction solution was filtered
  2. customdirectly loaded onto a column for purification by reverse phase high performance liquid chromatography

出典と根拠

ORDレコード
ord-5d9548b54cd34f82a6df6fb63df6ef62
出典データセット
uspto-grants-2009_04
特許番号
US07524847B2

反応ノート

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