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Sodium Hydroxide → HCID 49771573、化合物

HRID 1173944
ノート
印刷プレビュー

反応式

HRID 1173944 の反応式
C(N(CCC)[C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12](=[O:27])[C:13]2[CH:18]=[CH:17][C:16]([CH2:19][NH:20][CH2:21][C:22]3[NH:23][CH:24]=[CH:25][N:26]=3)=[CH:15][CH:14]=2)=[CH:7][CH:6]=1)CC.[CH2:31]([N:34]1[CH:38]=[CH:37][N:36]=[C:35]1[CH:39]=O)[CH2:32][CH3:33].[C:41]([BH3-])#[N:42].[Na+].[OH-].[Na+]>CO.C(O)(=O)C>[CH2:6]([N:42]([CH2:41][C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12](=[O:27])[C:13]2[CH:14]=[CH:15][C:16]([CH2:19][N:20]([CH2:21][C:22]3[NH:26][CH:25]=[CH:24][N:23]=3)[CH2:39][C:35]3[N:34]([CH2:31][CH2:32][CH3:33])[CH:38]=[CH:37][N:36]=3)=[CH:17][CH:18]=2)=[CH:7][CH:6]=1)[CH2:7][CH2:8][CH3:9])[CH2:5][CH3:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 14798Sodium HydroxideHCID 47776601-Propyl-1H-imidazole-2-carbaldehydeHCID 5003444Sodium cyanoborohydrideHCID 21084514N-[4-(dipropylamino)phenyl]-4-[(1H-imidazol-2-ylmethylamino)methyl]benzamide

生成物 1

HCID 49771573HCID 49771573、化合物

試薬・触媒・溶媒 2

HCID 176
Acetic Acid
溶媒
HCID 887Methanol溶媒

実験手順

The compound (120 mg) obtained in Example 47-3 was dissolved in methanol (5.0 ml) and then added with the compound (57.0 mg) obtained in Example 91-1 and sodium cyanoborohydride (18.0 mg). Then, the solution was adjusted to pH 5 with acetic acid and then stirred at room temperature for 2 days. After completion of the reaction, a 1 mol/l sodium hydroxide aqueous solution was added to the reaction solution, followed by separation/extraction with chloroform. The organic layer was dried with anhydrous sodium sulfate and the solvent was then distilled off. The residue was purified through silica gel column chromatography (chloroform/methanol) and then treated with hydrochloric acid, thereby obtaining hydrochloride (201 mg) of the subject compound as a white solid.

後処理

  1. customAfter completion of the reaction
  2. extractionfollowed by separation/extraction with chloroform
  3. dry with materialThe organic layer was dried with anhydrous sodium sulfate
  4. distillationthe solvent was then distilled off
  5. customThe residue was purified through silica gel column chromatography (chloroform/methanol)
  6. additiontreated with hydrochloric acid

出典と根拠

ORDレコード
ord-b03ce177e3e340faac34b1f720f5aabc
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07833991B2

反応ノート

読み込み中…

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